中国药学杂志

No.	Enterprise	Batch number number	Source(in Chinese)	No.	Enterprise	Batch number	Source(in Chinese)
H1	Q1	19015202	Lanzhou(兰州)	H27	Q5	20221223	Tianjin(天津)
H2		22015043	Xingtai(邢台)	H28		20230226	Changchun(长春)
H3		22015056	Beijing(北京)	H29		20230334	Shanghai(上海)
H4		22015090	Xi'an(西安)	H30		20230343	Shijiazhuang(石家庄)
H5		22015091	Xingtai(邢台)	H31		20230501	Jinan(济南)
H6		21015100	Chengdu(成都)	H32		20230504	Yichun(宜春)
H7		22015148	Taiyuan(太原)	H33		20230507	Haerbin(哈尔滨)
H8		22015149	Luohe(洛阳)	H34	Q6	121010	Tianjin(天津)
H9		22015150	Zhengzhou(郑州)	H35		122003	Shuozhou(朔州)
H10		22015151	Beijing(北京)	H36		123002	Taiyuan(太原)
H11		21015187	Chongqing(重庆)	H37	Q7	2220305	Fuyang(阜阳)
H12		21015395	Qingdao(青岛)	H38		2220305	Fuyang(阜阳)
H13	Q2	131065	Jinan(济南)	H39		2220902	Beijing(北京)
H14		131065	Changsha(长沙)	H40	Q8	20210680	Mianyang(绵阳)
H15		131069	Fuyang(阜阳)	H41		20210680	Zhengzhou(郑州)
H16		131069	Heze(菏泽)	H42		20220102	Changzhi(长治)
H17		131069	Yichun(宜春)	H43	Q9	220401	Zhengzhou(郑州)
H18		131070	Dezhou(德州)	H44		230501	Zhengzhou(郑州)
H19	Q3	210401	Changchun(长春)	H45		230501	Kaifeng(开封)
H20		211201	Handan(邯郸)	H46	Q10	WJ21056	Haerbin(哈尔滨)
H21		220701	Anshan(鞍山)	H47		WJ21057	Zhengzhou(郑州)
H22		220701	Yichun(宜春)	H48		WJ22115	Chengdu(成都)
H23	Q4	20220572	Chaoyang(朝阳)	H49	Q11	20211217	Kunming(昆明)
H24		20221221	Hengyang(衡阳)	H50		20230638	Shaoguan(韶关)
H25		20230411	Guangzhou(广州)	H51		20230638	Shaoguan(韶关)
H26		20230412	Wuhan(武汉)

No.	Enterprise	Batch number number	Source(in Chinese)	No.	Enterprise	Batch number	Source(in Chinese)
H1	Q1	19015202	Lanzhou(兰州)	H27	Q5	20221223	Tianjin(天津)
H2		22015043	Xingtai(邢台)	H28		20230226	Changchun(长春)
H3		22015056	Beijing(北京)	H29		20230334	Shanghai(上海)
H4		22015090	Xi'an(西安)	H30		20230343	Shijiazhuang(石家庄)
H5		22015091	Xingtai(邢台)	H31		20230501	Jinan(济南)
H6		21015100	Chengdu(成都)	H32		20230504	Yichun(宜春)
H7		22015148	Taiyuan(太原)	H33		20230507	Haerbin(哈尔滨)
H8		22015149	Luohe(洛阳)	H34	Q6	121010	Tianjin(天津)
H9		22015150	Zhengzhou(郑州)	H35		122003	Shuozhou(朔州)
H10		22015151	Beijing(北京)	H36		123002	Taiyuan(太原)
H11		21015187	Chongqing(重庆)	H37	Q7	2220305	Fuyang(阜阳)
H12		21015395	Qingdao(青岛)	H38		2220305	Fuyang(阜阳)
H13	Q2	131065	Jinan(济南)	H39		2220902	Beijing(北京)
H14		131065	Changsha(长沙)	H40	Q8	20210680	Mianyang(绵阳)
H15		131069	Fuyang(阜阳)	H41		20210680	Zhengzhou(郑州)
H16		131069	Heze(菏泽)	H42		20220102	Changzhi(长治)
H17		131069	Yichun(宜春)	H43	Q9	220401	Zhengzhou(郑州)
H18		131070	Dezhou(德州)	H44		230501	Zhengzhou(郑州)
H19	Q3	210401	Changchun(长春)	H45		230501	Kaifeng(开封)
H20		211201	Handan(邯郸)	H46	Q10	WJ21056	Haerbin(哈尔滨)
H21		220701	Anshan(鞍山)	H47		WJ21057	Zhengzhou(郑州)
H22		220701	Yichun(宜春)	H48		WJ22115	Chengdu(成都)
H23	Q4	20220572	Chaoyang(朝阳)	H49	Q11	20211217	Kunming(昆明)
H24		20221221	Hengyang(衡阳)	H50		20230638	Shaoguan(韶关)
H25		20230411	Guangzhou(广州)	H51		20230638	Shaoguan(韶关)
H26		20230412	Wuhan(武汉)

Componnet	Regression equation	Linearity range/μg·mL^-1	r
Chlorogenic acid	Y=1.21×10⁴X-2.35×10⁴	4.10	-65.60	0.998 9
Vanillic acid	Y=2.15×10⁴X-1.98×10³	0.54	-8.60	0.998 0
Hyperoside	Y=8.47×10³X-2.87×10³	1.84	-29.40	0.999 0
Isochlorogenic acid B	Y=1.43×10⁴X-2.78×10³	0.81	-12.93	0.998 9
Isochlorogenic acid A	Y=1.62×10⁴X-8.87×10³	1.36	-21.80	0.999 1

Componnet	Regression equation	Linearity range/μg·mL^-1	r
Chlorogenic acid	Y=1.21×10⁴X-2.35×10⁴	4.10	-65.60	0.998 9
Vanillic acid	Y=2.15×10⁴X-1.98×10³	0.54	-8.60	0.998 0
Hyperoside	Y=8.47×10³X-2.87×10³	1.84	-29.40	0.999 0
Isochlorogenic acid B	Y=1.43×10⁴X-2.78×10³	0.81	-12.93	0.998 9
Isochlorogenic acid A	Y=1.62×10⁴X-8.87×10³	1.36	-21.80	0.999 1

Componnet	m(Original)/μg	m(Sample)/g	m(Added)/μg	m(Measured)/μg	Recovery/%	Average recovery/%	RSD/%
Chlorogenic acid	81.822 2	0.502 0	82.000 0	157.011 9	91.69	98.09	4.07
	82.474 2	0.506 0	82.000 0	162.548 3	97.65
	81.659 2	0.501 0	82.000 0	160.455 4	96.09
	82.148 2	0.504 0	82.000 0	163.511 8	99.22
	81.903 7	0.502 5	82.000 0	166.584 9	103.27
	81.985 2	0.503 0	82.000 0	164.485 6	100.61
Vanillic acid	9.866 9	0.502 0	9.672 3	20.334 6	108.22	107.15	3.69
	9.945 5	0.506 0	9.672 3	20.425 0	108.35
	9.847 2	0.501 0	9.672 3	20.126 3	106.27
	9.906 2	0.504 0	9.672 3	20.575 9	110.31
	9.876 7	0.502 5	9.672 3	20.524 5	110.08
	9.886 5	0.503 0	9.672 3	19.524 2	99.64
Hyperoside	58.402 9	0.502 0	57.871 8	122.516 4	110.79	109.35	3.65
	58.868 2	0.506 0	57.871 8	118.429 6	102.92
	58.286 5	0.501 0	57.871 8	124.197 1	113.89
	58.635 5	0.504 0	57.871 8	120.332 2	106.61
	58.461 0	0.502 5	57.871 8	121.960 2	109.72
	58.519 2	0.503 0	57.871 8	123.426 4	112.16
Isochlorogenic acid B	9.323 1	0.502 0	9.382 5	18.202 4	94.64	96.27	3.92
	9.397 3	0.506 0	9.382 5	18.978 0	102.11
	9.304 5	0.501 0	9.382 5	18.338 6	96.29
	9.360 2	0.504 0	9.382 5	17.867 5	90.67
	9.332 3	0.502 5	9.382 5	18.528 1	98.01
	9.341 6	0.503 0	9.382 5	18.337 8	95.88
Isochlorogenic acid A	17.902 5	0.502 0	17.351 5	36.739 2	108.56	105.27	2.83
	18.045 1	0.506 0	17.351 5	35.629 9	101.34
	17.866 8	0.501 0	17.351 5	36.405 2	106.84
	17.973 8	0.504 0	17.351 5	36.718 2	108.03
	17.920 3	0.502 5	17.351 5	35.735 6	102.67
	17.938 2	0.503 0	17.351 5	36.010 0	104.15

Componnet	m(Original)/μg	m(Sample)/g	m(Added)/μg	m(Measured)/μg	Recovery/%	Average recovery/%	RSD/%
Chlorogenic acid	81.822 2	0.502 0	82.000 0	157.011 9	91.69	98.09	4.07
	82.474 2	0.506 0	82.000 0	162.548 3	97.65
	81.659 2	0.501 0	82.000 0	160.455 4	96.09
	82.148 2	0.504 0	82.000 0	163.511 8	99.22
	81.903 7	0.502 5	82.000 0	166.584 9	103.27
	81.985 2	0.503 0	82.000 0	164.485 6	100.61
Vanillic acid	9.866 9	0.502 0	9.672 3	20.334 6	108.22	107.15	3.69
	9.945 5	0.506 0	9.672 3	20.425 0	108.35
	9.847 2	0.501 0	9.672 3	20.126 3	106.27
	9.906 2	0.504 0	9.672 3	20.575 9	110.31
	9.876 7	0.502 5	9.672 3	20.524 5	110.08
	9.886 5	0.503 0	9.672 3	19.524 2	99.64
Hyperoside	58.402 9	0.502 0	57.871 8	122.516 4	110.79	109.35	3.65
	58.868 2	0.506 0	57.871 8	118.429 6	102.92
	58.286 5	0.501 0	57.871 8	124.197 1	113.89
	58.635 5	0.504 0	57.871 8	120.332 2	106.61
	58.461 0	0.502 5	57.871 8	121.960 2	109.72
	58.519 2	0.503 0	57.871 8	123.426 4	112.16
Isochlorogenic acid B	9.323 1	0.502 0	9.382 5	18.202 4	94.64	96.27	3.92
	9.397 3	0.506 0	9.382 5	18.978 0	102.11
	9.304 5	0.501 0	9.382 5	18.338 6	96.29
	9.360 2	0.504 0	9.382 5	17.867 5	90.67
	9.332 3	0.502 5	9.382 5	18.528 1	98.01
	9.341 6	0.503 0	9.382 5	18.337 8	95.88
Isochlorogenic acid A	17.902 5	0.502 0	17.351 5	36.739 2	108.56	105.27	2.83
	18.045 1	0.506 0	17.351 5	35.629 9	101.34
	17.866 8	0.501 0	17.351 5	36.405 2	106.84
	17.973 8	0.504 0	17.351 5	36.718 2	108.03
	17.920 3	0.502 5	17.351 5	35.735 6	102.67
	17.938 2	0.503 0	17.351 5	36.010 0	104.15

No.	Chlorogenic acid	Vanillic acid	Hyperoside	Isochlorogenic acid B	Isochlorogenic acid A	No.	Chlorogenic acid	Vanillic acid	Hyperos ide	Isochlorogenic acid B	Isochlorogenic acid A
H1	0.104 2	0.024 1	0.097 6	0.020 5	0.039 7	H27	0.147 1	0.019 2	0.127 3	0.031 5	0.053 8
H2	0.153 4	0.021 7	0.145 7	0.035 0	0.047 5	H28	0.199 2	0.023 0	0.120 8	0.026 0	0.046 4
H3	0.156 0	0.023 4	0.129 5	0.026 9	0.043 1	H29	0.205 9	0.028 2	0.146 8	0.039 7	0.055 0
H4	0.152 2	0.021 7	0.121 1	0.021 5	0.032 9	H30	0.193 6	0.036 2	0.162 4	0.027 1	0.045 8
H5	0.154 1	0.021 7	0.118 7	0.025 7	0.044 3	H31	0.205 6	0.031 9	0.174 1	0.041 4	0.058 3
H6	0.094 5	0.018 6	0.078 7	0.013 3	0.028 9	H32	0.178 2	0.022 1	0.132 6	0.027 3	0.042 4
H7	0.148 0	0.023 4	0.134 7	0.023 9	0.038 2	H33	0.206 0	0.034 6	0.163 4	0.021 7	0.040 1
H8	0.149 1	0.022 7	0.145 2	0.039 3	0.044 6	H34	0.085 8	0.016 5	0.113 4	0.021 4	0.030 1
H9	0.148 6	0.021 7	0.133 9	0.036 7	0.050 6	H35	0.088 1	0.014 9	0.106 3	0.020 6	0.026 0
H10	0.154 4	0.023 1	0.139 0	0.026 4	0.038 3	H36	0.173 8	0.029 0	0.133 5	0.020 2	0.033 2
H11	0.118 2	0.016 7	0.100 8	0.014 8	0.027 4	H37	0.129 7	0.019 6	0.078 3	0.014 6	0.047 3
H12	0.184 1	0.023 7	0.113 6	0.025 1	0.043 0	H38	0.130 0	0.019 2	0.085 2	0.026 4	0.064 5
H13	0.227 0	0.023 2	0.226 1	0.034 3	0.021 7	H39	0.053 6	0.014 5	0.098 7	0.017 6	0.046 4
H14	0.189 4	0.019 2	0.214 4	0.032 9	0.022 4	H40	0.122 8	0.011 7	0.060 1	0.015 6	0.034 1
H15	0.205 9	0.031 0	0.370 2	0.063 2	0.037 1	H41	0.118 9	0.012 2	0.056 9	0.013 3	0.027 2
H16	0.200 8	0.021 3	0.353 9	0.057 0	0.029 3	H42	0.097 1	0.009 7	0.097 5	0.018 1	0.026 7
H17	0.192 6	0.021 9	0.341 4	0.057 6	0.037 9	H43	0.093 3	0.013 3	0.023 0	0.006 6	0.041 4
H18	0.206 9	0.031 4	0.363 6	0.057 3	0.033 0	H44	0.081 0	0.012 1	0.028 9	0.009 6	0.042 1
H19	0.135 2	0.016 9	0.110 7	0.017 8	0.035 9	H45	0.084 7	0.015 5	0.032 7	0.011 1	0.043 8
H20	0.121 9	0.021 0	0.109 7	0.020 7	0.037 6	H46	0.077 5	0.018 3	0.031 2	0.017 9	0.056 8
H21	0.135 7	0.021 3	0.104 9	0.026 4	0.045 3	H47	0.067 9	0.016 8	0.032 3	0.016 6	0.047 1
H22	0.131 4	0.021 5	0.088 9	0.020 2	0.040 0	H48	0.063 5	0.019 6	0.036 7	0.014 8	0.056 4
H23	0.133 5	0.022 7	0.026 2	0.009 6	0.042 4	H49	0.053 8	0.018 0	0.036 4	0.009 1	0.043 5
H24	0.117 2	0.023 9	0.027 8	0.010 5	0.041 5	H50	0.047 2	0.016 9	0.035 5	0.006 4	0.053 8
H25	0.116 9	0.018 8	0.038 0	0.010 8	0.049 8	H51	0.056 4	0.018 4	0.034 0	0.006 5	0.053 0
H26	0.118 0	0.018 1	0.042 1	0.008 7	0.043 1

No.	Chlorogenic acid	Vanillic acid	Hyperoside	Isochlorogenic acid B	Isochlorogenic acid A	No.	Chlorogenic acid	Vanillic acid	Hyperos ide	Isochlorogenic acid B	Isochlorogenic acid A
H1	0.104 2	0.024 1	0.097 6	0.020 5	0.039 7	H27	0.147 1	0.019 2	0.127 3	0.031 5	0.053 8
H2	0.153 4	0.021 7	0.145 7	0.035 0	0.047 5	H28	0.199 2	0.023 0	0.120 8	0.026 0	0.046 4
H3	0.156 0	0.023 4	0.129 5	0.026 9	0.043 1	H29	0.205 9	0.028 2	0.146 8	0.039 7	0.055 0
H4	0.152 2	0.021 7	0.121 1	0.021 5	0.032 9	H30	0.193 6	0.036 2	0.162 4	0.027 1	0.045 8
H5	0.154 1	0.021 7	0.118 7	0.025 7	0.044 3	H31	0.205 6	0.031 9	0.174 1	0.041 4	0.058 3
H6	0.094 5	0.018 6	0.078 7	0.013 3	0.028 9	H32	0.178 2	0.022 1	0.132 6	0.027 3	0.042 4
H7	0.148 0	0.023 4	0.134 7	0.023 9	0.038 2	H33	0.206 0	0.034 6	0.163 4	0.021 7	0.040 1
H8	0.149 1	0.022 7	0.145 2	0.039 3	0.044 6	H34	0.085 8	0.016 5	0.113 4	0.021 4	0.030 1
H9	0.148 6	0.021 7	0.133 9	0.036 7	0.050 6	H35	0.088 1	0.014 9	0.106 3	0.020 6	0.026 0
H10	0.154 4	0.023 1	0.139 0	0.026 4	0.038 3	H36	0.173 8	0.029 0	0.133 5	0.020 2	0.033 2
H11	0.118 2	0.016 7	0.100 8	0.014 8	0.027 4	H37	0.129 7	0.019 6	0.078 3	0.014 6	0.047 3
H12	0.184 1	0.023 7	0.113 6	0.025 1	0.043 0	H38	0.130 0	0.019 2	0.085 2	0.026 4	0.064 5
H13	0.227 0	0.023 2	0.226 1	0.034 3	0.021 7	H39	0.053 6	0.014 5	0.098 7	0.017 6	0.046 4
H14	0.189 4	0.019 2	0.214 4	0.032 9	0.022 4	H40	0.122 8	0.011 7	0.060 1	0.015 6	0.034 1
H15	0.205 9	0.031 0	0.370 2	0.063 2	0.037 1	H41	0.118 9	0.012 2	0.056 9	0.013 3	0.027 2
H16	0.200 8	0.021 3	0.353 9	0.057 0	0.029 3	H42	0.097 1	0.009 7	0.097 5	0.018 1	0.026 7
H17	0.192 6	0.021 9	0.341 4	0.057 6	0.037 9	H43	0.093 3	0.013 3	0.023 0	0.006 6	0.041 4
H18	0.206 9	0.031 4	0.363 6	0.057 3	0.033 0	H44	0.081 0	0.012 1	0.028 9	0.009 6	0.042 1
H19	0.135 2	0.016 9	0.110 7	0.017 8	0.035 9	H45	0.084 7	0.015 5	0.032 7	0.011 1	0.043 8
H20	0.121 9	0.021 0	0.109 7	0.020 7	0.037 6	H46	0.077 5	0.018 3	0.031 2	0.017 9	0.056 8
H21	0.135 7	0.021 3	0.104 9	0.026 4	0.045 3	H47	0.067 9	0.016 8	0.032 3	0.016 6	0.047 1
H22	0.131 4	0.021 5	0.088 9	0.020 2	0.040 0	H48	0.063 5	0.019 6	0.036 7	0.014 8	0.056 4
H23	0.133 5	0.022 7	0.026 2	0.009 6	0.042 4	H49	0.053 8	0.018 0	0.036 4	0.009 1	0.043 5
H24	0.117 2	0.023 9	0.027 8	0.010 5	0.041 5	H50	0.047 2	0.016 9	0.035 5	0.006 4	0.053 8
H25	0.116 9	0.018 8	0.038 0	0.010 8	0.049 8	H51	0.056 4	0.018 4	0.034 0	0.006 5	0.053 0
H26	0.118 0	0.018 1	0.042 1	0.008 7	0.043 1

Batch No.	t1	t2	t3	t4	t5	t6	t7	t8	t9	t10	t11	t12	t13	t14	t15	t16
H1	0.394	0.472	0.647	0.715	1.000	1.101	1.846	1.876	1.977	2.035	2.072	2.605	3.454	3.766	3.842	3.904
H2	0.393	0.474	0.650	0.719	1.000	1.100	1.828	1.858	1.958	2.016	2.053	2.580	3.424	3.734	3.809	3.871
H3	0.394	0.473	0.649	0.714	1.000	1.100	1.838	1.868	1.969	2.027	2.065	2.597	3.452	3.767	3.843	3.906
H4	0.392	0.471	0.648	0.716	1.000	1.101	1.834	1.865	1.966	2.025	2.062	2.596	3.452	3.767	3.843	3.905
H5	0.391	0.472	0.648	0.716	1.000	1.100	1.832	1.863	1.963	2.023	2.060	2.594	3.450	3.764	3.840	3.904
H6	0.391	0.472	0.649	0.716	1.000	1.100	1.832	1.864	1.965	2.025	2.063	2.595	3.452	3.767	3.844	3.906
H7	0.391	0.471	0.648	0.716	1.000	1.100	1.831	1.861	1.962	2.023	2.060	2.592	3.445	3.758	3.834	3.898
H8	0.393	0.472	0.650	0.716	1.000	1.100	1.835	1.866	1.969	2.027	2.065	2.596	3.451	3.765	3.841	3.904
H9	0.394	0.473	0.650	0.719	1.000	1.101	1.831	1.861	1.962	2.021	2.059	2.589	3.443	3.757	3.833	3.898
H10	0.389	0.467	0.647	0.714	1.000	1.101	1.834	1.864	1.966	2.026	2.064	2.599	3.454	3.771	3.847	3.912
H11	0.385	0.469	0.647	0.715	1.000	1.102	1.838	1.869	1.973	2.032	2.070	2.610	3.467	3.784	3.861	3.925
H12	0.389	0.469	0.647	0.714	1.000	1.101	1.833	1.863	1.965	2.024	2.062	2.594	3.447	3.759	3.836	3.899
H13	0.386	0.466	0.649	0.713	1.000	1.101	1.844	1.875	1.979	2.038	2.078	2.620	3.486	3.804	3.882	3.946
H14	0.386	0.469	0.648	0.711	1.000	1.102	1.849	1.880	1.985	2.044	2.082	2.622	3.482	3.800	3.879	3.942
H15	0.386	0.466	0.649	0.713	1.000	1.101	1.842	1.873	1.978	2.039	2.077	2.616	3.484	3.798	3.877	3.940
H16	0.389	0.463	0.647	0.714	1.000	1.101	1.836	1.867	1.970	2.028	2.066	2.602	3.458	3.774	3.851	3.914
H17	0.391	0.468	0.648	0.714	1.000	1.102	1.838	1.870	1.974	2.035	2.071	2.611	3.474	3.789	3.868	3.931
H18	0.398	0.473	0.662	0.732	1.000	1.121	1.863	1.894	1.998	2.057	2.096	2.636	3.500	3.818	3.897	3.962
H19	0.389	0.472	0.648	0.716	1.000	1.099	1.826	1.856	1.959	2.019	2.056	2.588	3.445	3.762	3.838	3.899
H20	0.393	0.475	0.654	0.720	1.000	1.104	1.839	1.870	1.972	2.032	2.070	2.600	3.458	3.775	3.852	3.914
H21	0.395	0.476	0.653	0.719	1.000	1.103	1.841	1.872	1.975	2.034	2.071	2.608	3.468	3.787	3.864	3.926
H22	0.388	0.473	0.651	0.717	1.000	1.103	1.834	1.864	1.968	2.027	2.064	2.597	3.456	3.775	3.851	3.914
H23	0.390	0.474	0.653	0.719	1.000	1.102	1.834	1.865	1.964	2.025	2.064	2.598	3.453	3.772	3.849	3.912
H24	0.391	0.474	0.652	0.718	1.000	1.103	1.832	1.864	1.967	2.025	2.062	2.596	3.452	3.770	3.846	3.909
H25	0.390	0.474	0.654	0.720	1.000	1.102	1.827	1.857	1.961	2.019	2.058	2.588	3.441	3.757	3.834	3.898
H26	0.390	0.474	0.654	0.721	1.000	1.103	1.832	1.863	1.962	2.023	2.060	2.594	3.452	3.769	3.846	3.908
H27	0.391	0.475	0.653	0.717	1.000	1.103	1.830	1.861	1.964	2.025	2.063	2.600	3.463	3.791	3.867	3.927
H28	0.390	0.475	0.653	0.716	1.000	1.103	1.833	1.864	1.968	2.029	2.067	2.604	3.469	3.798	3.874	3.936
H29	0.389	0.474	0.654	0.718	1.000	1.101	1.832	1.863	1.969	2.029	2.067	2.607	3.471	3.802	3.879	3.942
H30	0.390	0.474	0.654	0.718	1.000	1.101	1.834	1.865	1.970	2.031	2.069	2.607	3.472	3.803	3.880	3.943
H31	0.389	0.474	0.652	0.717	1.000	1.101	1.831	1.862	1.965	2.026	2.064	2.599	3.459	3.788	3.863	3.923
H32	0.389	0.473	0.650	0.716	1.000	1.101	1.831	1.862	1.965	2.026	2.064	2.599	3.461	3.790	3.867	3.930
H33	0.389	0.474	0.653	0.719	1.000	1.101	1.829	1.860	1.962	2.023	2.061	2.593	3.451	3.778	3.853	3.915
H34	0.389	0.474	0.652	0.713	1.000	1.103	1.835	1.866	1.969	2.031	2.068	2.603	3.464	3.794	3.870	3.932
H35	0.385	0.470	0.648	0.712	1.000	1.097	1.826	1.859	1.966	2.025	2.063	2.603	3.471	3.802	3.877	3.937
H36	0.388	0.471	0.652	0.716	1.000	1.103	1.830	1.862	1.966	2.027	2.065	2.604	3.470	3.801	3.876	3.938
H37	0.384	0.469	0.651	0.714	1.000	1.103	1.834	1.866	1.971	2.032	2.070	2.607	3.474	3.804	3.879	3.942
H38	0.392	0.475	0.655	0.718	1.000	1.104	1.830	1.861	1.964	2.025	2.063	2.597	3.456	3.785	3.860	3.921
H39	0.389	0.475	0.655	0.720	1.000	1.104	1.830	1.861	1.966	2.025	2.063	2.596	3.456	3.784	3.858	3.919
H40	0.391	0.475	0.656	0.719	1.000	1.103	1.828	1.859	1.962	2.023	2.060	2.593	3.451	3.776	3.852	3.914
H41	0.389	0.474	0.655	0.718	1.000	1.105	1.831	1.863	1.947	2.028	2.066	2.601	3.460	3.788	3.862	3.925
H42	0.390	0.474	0.654	0.719	1.000	1.103	1.828	1.860	1.963	2.023	2.060	2.593	3.449	3.776	3.852	3.911
H43	0.385	0.473	0.661	0.717	1.000	1.104	1.834	1.866	1.972	2.029	2.069	2.605	3.469	3.799	3.875	3.936
H44	0.388	0.474	0.661	0.718	1.000	1.104	1.831	1.862	1.973	2.028	2.066	2.602	3.464	3.792	3.870	3.930
H45	0.386	0.473	0.653	0.718	1.000	1.102	1.831	1.863	1.971	2.027	2.066	2.605	3.467	3.798	3.873	3.938
H46	0.385	0.472	0.652	0.715	1.000	1.102	1.835	1.867	1.971	2.030	2.069	2.604	3.463	3.795	3.870	3.934
H47	0.386	0.472	0.652	0.714	1.000	1.102	1.833	1.864	1.970	2.027	2.066	2.599	3.462	3.791	3.866	3.931
H48	0.385	0.472	0.652	0.717	1.000	1.102	1.835	1.866	1.973	2.028	2.068	2.603	3.464	3.792	3.867	3.933
H49	0.383	0.472	0.652	0.716	1.000	1.103	1.830	1.863	1.970	2.026	2.066	2.602	3.463	3.793	3.867	3.933
H50	0.385	0.472	0.651	0.716	1.000	1.101	1.831	1.863	1.966	2.024	2.064	2.599	3.461	3.790	3.865	3.930
H51	0.383	0.471	0.651	0.717	1.000	1.102	1.826	1.858	1.961	2.020	2.061	2.596	3.455	3.784	3.859	3.923
RSD/%	0.831	0.581	0.548	0.436	0.000	0.284	0.342	0.336	0.375	0.328	0.331	0.354	0.370	0.438	0.434	0.430

Batch No.	t1	t2	t3	t4	t5	t6	t7	t8	t9	t10	t11	t12	t13	t14	t15	t16
H1	0.394	0.472	0.647	0.715	1.000	1.101	1.846	1.876	1.977	2.035	2.072	2.605	3.454	3.766	3.842	3.904
H2	0.393	0.474	0.650	0.719	1.000	1.100	1.828	1.858	1.958	2.016	2.053	2.580	3.424	3.734	3.809	3.871
H3	0.394	0.473	0.649	0.714	1.000	1.100	1.838	1.868	1.969	2.027	2.065	2.597	3.452	3.767	3.843	3.906
H4	0.392	0.471	0.648	0.716	1.000	1.101	1.834	1.865	1.966	2.025	2.062	2.596	3.452	3.767	3.843	3.905
H5	0.391	0.472	0.648	0.716	1.000	1.100	1.832	1.863	1.963	2.023	2.060	2.594	3.450	3.764	3.840	3.904
H6	0.391	0.472	0.649	0.716	1.000	1.100	1.832	1.864	1.965	2.025	2.063	2.595	3.452	3.767	3.844	3.906
H7	0.391	0.471	0.648	0.716	1.000	1.100	1.831	1.861	1.962	2.023	2.060	2.592	3.445	3.758	3.834	3.898
H8	0.393	0.472	0.650	0.716	1.000	1.100	1.835	1.866	1.969	2.027	2.065	2.596	3.451	3.765	3.841	3.904
H9	0.394	0.473	0.650	0.719	1.000	1.101	1.831	1.861	1.962	2.021	2.059	2.589	3.443	3.757	3.833	3.898
H10	0.389	0.467	0.647	0.714	1.000	1.101	1.834	1.864	1.966	2.026	2.064	2.599	3.454	3.771	3.847	3.912
H11	0.385	0.469	0.647	0.715	1.000	1.102	1.838	1.869	1.973	2.032	2.070	2.610	3.467	3.784	3.861	3.925
H12	0.389	0.469	0.647	0.714	1.000	1.101	1.833	1.863	1.965	2.024	2.062	2.594	3.447	3.759	3.836	3.899
H13	0.386	0.466	0.649	0.713	1.000	1.101	1.844	1.875	1.979	2.038	2.078	2.620	3.486	3.804	3.882	3.946
H14	0.386	0.469	0.648	0.711	1.000	1.102	1.849	1.880	1.985	2.044	2.082	2.622	3.482	3.800	3.879	3.942
H15	0.386	0.466	0.649	0.713	1.000	1.101	1.842	1.873	1.978	2.039	2.077	2.616	3.484	3.798	3.877	3.940
H16	0.389	0.463	0.647	0.714	1.000	1.101	1.836	1.867	1.970	2.028	2.066	2.602	3.458	3.774	3.851	3.914
H17	0.391	0.468	0.648	0.714	1.000	1.102	1.838	1.870	1.974	2.035	2.071	2.611	3.474	3.789	3.868	3.931
H18	0.398	0.473	0.662	0.732	1.000	1.121	1.863	1.894	1.998	2.057	2.096	2.636	3.500	3.818	3.897	3.962
H19	0.389	0.472	0.648	0.716	1.000	1.099	1.826	1.856	1.959	2.019	2.056	2.588	3.445	3.762	3.838	3.899
H20	0.393	0.475	0.654	0.720	1.000	1.104	1.839	1.870	1.972	2.032	2.070	2.600	3.458	3.775	3.852	3.914
H21	0.395	0.476	0.653	0.719	1.000	1.103	1.841	1.872	1.975	2.034	2.071	2.608	3.468	3.787	3.864	3.926
H22	0.388	0.473	0.651	0.717	1.000	1.103	1.834	1.864	1.968	2.027	2.064	2.597	3.456	3.775	3.851	3.914
H23	0.390	0.474	0.653	0.719	1.000	1.102	1.834	1.865	1.964	2.025	2.064	2.598	3.453	3.772	3.849	3.912
H24	0.391	0.474	0.652	0.718	1.000	1.103	1.832	1.864	1.967	2.025	2.062	2.596	3.452	3.770	3.846	3.909
H25	0.390	0.474	0.654	0.720	1.000	1.102	1.827	1.857	1.961	2.019	2.058	2.588	3.441	3.757	3.834	3.898
H26	0.390	0.474	0.654	0.721	1.000	1.103	1.832	1.863	1.962	2.023	2.060	2.594	3.452	3.769	3.846	3.908
H27	0.391	0.475	0.653	0.717	1.000	1.103	1.830	1.861	1.964	2.025	2.063	2.600	3.463	3.791	3.867	3.927
H28	0.390	0.475	0.653	0.716	1.000	1.103	1.833	1.864	1.968	2.029	2.067	2.604	3.469	3.798	3.874	3.936
H29	0.389	0.474	0.654	0.718	1.000	1.101	1.832	1.863	1.969	2.029	2.067	2.607	3.471	3.802	3.879	3.942
H30	0.390	0.474	0.654	0.718	1.000	1.101	1.834	1.865	1.970	2.031	2.069	2.607	3.472	3.803	3.880	3.943
H31	0.389	0.474	0.652	0.717	1.000	1.101	1.831	1.862	1.965	2.026	2.064	2.599	3.459	3.788	3.863	3.923
H32	0.389	0.473	0.650	0.716	1.000	1.101	1.831	1.862	1.965	2.026	2.064	2.599	3.461	3.790	3.867	3.930
H33	0.389	0.474	0.653	0.719	1.000	1.101	1.829	1.860	1.962	2.023	2.061	2.593	3.451	3.778	3.853	3.915
H34	0.389	0.474	0.652	0.713	1.000	1.103	1.835	1.866	1.969	2.031	2.068	2.603	3.464	3.794	3.870	3.932
H35	0.385	0.470	0.648	0.712	1.000	1.097	1.826	1.859	1.966	2.025	2.063	2.603	3.471	3.802	3.877	3.937
H36	0.388	0.471	0.652	0.716	1.000	1.103	1.830	1.862	1.966	2.027	2.065	2.604	3.470	3.801	3.876	3.938
H37	0.384	0.469	0.651	0.714	1.000	1.103	1.834	1.866	1.971	2.032	2.070	2.607	3.474	3.804	3.879	3.942
H38	0.392	0.475	0.655	0.718	1.000	1.104	1.830	1.861	1.964	2.025	2.063	2.597	3.456	3.785	3.860	3.921
H39	0.389	0.475	0.655	0.720	1.000	1.104	1.830	1.861	1.966	2.025	2.063	2.596	3.456	3.784	3.858	3.919
H40	0.391	0.475	0.656	0.719	1.000	1.103	1.828	1.859	1.962	2.023	2.060	2.593	3.451	3.776	3.852	3.914
H41	0.389	0.474	0.655	0.718	1.000	1.105	1.831	1.863	1.947	2.028	2.066	2.601	3.460	3.788	3.862	3.925
H42	0.390	0.474	0.654	0.719	1.000	1.103	1.828	1.860	1.963	2.023	2.060	2.593	3.449	3.776	3.852	3.911
H43	0.385	0.473	0.661	0.717	1.000	1.104	1.834	1.866	1.972	2.029	2.069	2.605	3.469	3.799	3.875	3.936
H44	0.388	0.474	0.661	0.718	1.000	1.104	1.831	1.862	1.973	2.028	2.066	2.602	3.464	3.792	3.870	3.930
H45	0.386	0.473	0.653	0.718	1.000	1.102	1.831	1.863	1.971	2.027	2.066	2.605	3.467	3.798	3.873	3.938
H46	0.385	0.472	0.652	0.715	1.000	1.102	1.835	1.867	1.971	2.030	2.069	2.604	3.463	3.795	3.870	3.934
H47	0.386	0.472	0.652	0.714	1.000	1.102	1.833	1.864	1.970	2.027	2.066	2.599	3.462	3.791	3.866	3.931
H48	0.385	0.472	0.652	0.717	1.000	1.102	1.835	1.866	1.973	2.028	2.068	2.603	3.464	3.792	3.867	3.933
H49	0.383	0.472	0.652	0.716	1.000	1.103	1.830	1.863	1.970	2.026	2.066	2.602	3.463	3.793	3.867	3.933
H50	0.385	0.472	0.651	0.716	1.000	1.101	1.831	1.863	1.966	2.024	2.064	2.599	3.461	3.790	3.865	3.930
H51	0.383	0.471	0.651	0.717	1.000	1.102	1.826	1.858	1.961	2.020	2.061	2.596	3.455	3.784	3.859	3.923
RSD/%	0.831	0.581	0.548	0.436	0.000	0.284	0.342	0.336	0.375	0.328	0.331	0.354	0.370	0.438	0.434	0.430

Component	Initial eigenvalue	Extract the sum of squares of the load
1	5.716	35.725	35.725	5.716	35.725	35.725
2	3.417	21.353	57.078	3.417	21.353	57.078
3	1.519	9.493	66.572	1.519	9.493	66.572
4	1.462	9.137	75.709	1.462	9.137	75.709

Component	Initial eigenvalue	Extract the sum of squares of the load
1	5.716	35.725	35.725	5.716	35.725	35.725
2	3.417	21.353	57.078	3.417	21.353	57.078
3	1.519	9.493	66.572	1.519	9.493	66.572
4	1.462	9.137	75.709	1.462	9.137	75.709

基于HPLC指纹图谱结合多成分含量测定和化学模式识别的大山楂丸质量评价

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李运 ¹ , 王苗 ² , 刘晓玲 ² , 许晓辉 ¹ , 马海棠 ² , 戚鹏飞 ¹ , 邱国玉 ³ , 程显隆 ⁴^,^*

中国药学杂志 | 论著 2024,59(24): 2372-2383

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中国药学杂志 | 论著 2024, 59(24): 2372-2383

基于HPLC指纹图谱结合多成分含量测定和化学模式识别的大山楂丸质量评价

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李运¹, 王苗², 刘晓玲², 许晓辉¹, 马海棠², 戚鹏飞¹, 邱国玉³, 程显隆⁴^,^*

作者信息

¹ 兰州市食品药品检验检测研究院, 兰州 730050

² 甘肃中医药大学药学院, 兰州 730000

³ 甘肃药业集团科技创新研究院有限公司, 兰州 730000

⁴ 中国食品药品检定研究院, 北京 100050

李运,男,硕士,高级工程师研究方向:中药质量控制研究

通讯作者:

^* 程显隆,男,研究员研究方向:中药质量控制研究 Tel:(010)67095432

Quality Evaluation of Dashanzha Pills Based on HPLC Fingerprint and Multi-Component Analysis Combined with Chemical Pattern Recognition

Yun LI¹, Miao WANG², Xiaoling LIU², Xiaohui XU¹, Haitang MA², Pengfei QI¹, Guoyu QIU³, Xian-long CHENG⁴^,^*

Affiliations

¹ Lanzhou Institute for Food and Drug Control, Lanzhou 730050, China

² College of Pharmacy, Gansu University of Chinese Medicine, Lanzhou 730000, China

³ Gansu Pharmaceutical Group Science and Technology Innovation Research Institute Co., Ltd. Lanzhou 730000, China

⁴ National Institutes for Food and Drug Control, Beijing 100050, China

出版时间: 2024-12-22 doi: 10.11669/cpj.2024.24.010

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摘要

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目的建立大山楂丸(Dashanzha Pills,DSZP)的高效液相色谱(HPLC)指纹图谱及5种指标性成分的含量测定方法,并结合化学模式识别法对其质量进行评价。方法分析采用Eclipse Plus C₁₈色谱柱(4.6 mm×250 mm,5 μm),柱温30 ℃;以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,流速1.0 mL·min^-1,检测波长250 nm,进样量10 μL。基于51批次DSZP样本建立指纹图谱,指认了5种指标性成分,并对其进行了定量测定,结合聚类分析、主成分分析(principle component analysis,PCA)、正交偏最小二乘判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)等模式识别方法对DSZP进行综合分析。结果建立了DSZP指纹图谱,共标定了16个共有峰,并指认了5个化学成分,分别为绿原酸(5号峰)、香草酸(6号峰)、金丝桃苷(7号峰)、异绿原酸B(9号峰)、异绿原酸A(10号峰);含量测定5种指标性成分的线性关系良好(r>0.998),加标回收率在96.27%~109.35%,RSD在2.83%~4.07%。绿原酸、香草酸、金丝桃苷、异绿原酸 B、异绿原酸A的含量分别在0.047 2~0.227 0、0.009 7~0.036 2、0.023 0~0.370 2、0.006 4~0.0632和0.021 7~0.064 5 mg·g^-1之间。除厂家Q2外,其余厂家样品含量在各自均值的±30%,表明不同企业间的产品质量存在一定差异。化学模式识别结果提示,所有样品大致可分为两类,表明企业内的制备工艺较稳定,但企业间存在一定差异。筛选得到的样品差异标志物中包括指标成分绿原酸、金丝桃苷和异绿原酸B。。结论该定量方法准确、快速,可行性较高,结合化学模式识别可为DSZP的质量进行综合评价。

关键词

大山楂丸 / 高效液相色谱指纹图谱 / 化学模式识别 / 质量控制 / 金丝桃苷 / 异绿原酸B

Abstract

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OBJECTIVE To establish the HPLC fingerprints and content determination method of five index components of Dashanzha pills(DSZP), and evaluate the quality combined with chemical pattern recognition. METHODS The analysis was performed on an Eclipse plus C₁₈ column (4.6 mm×250 mm, 5 μm) at 30 ℃. Acetonitrile-0.1% formic acid aqueous solution was used as the mobile phase for gradient elution at flow rate of 1.0 mL·min^-1. The detection wavelength was set at 250 nm, and the injection volume was 10 μL. Based on 51 batches of DSZP samples, the fingerprint was established, and five index components were identified and quantitatively determined.Cluster analysis, principal component analysis and orthogonal partial least squares discriminant analysis were used to comprehensively analyze 51 batches of samples. RESULTS The fingerprints of DSZP were established, sixteen peaks were identified, and five chemical components were identified. They were chlorogenic acid (peak 5), vanillic acid (peak 6), hyperoside (peak 7), isochlorogenic acid B (peak 9), and isochlorogenic acid A (peak 10).The linear relationship of the five index components was good (r>0.998), and the recovery rate was 96.27%-109.35%, and the RSD was 2.83%-4.07%. The contents of chlorogenic acid, vanillicacid, hyperoside, isochlorogenic acid B, and isochlorogenic acid A were 0.047 2-0.227 0, 0.009 7-0.036 2, 0.023 0-0.370 2, 0.006 4-0.063 2 and 0.021 7-0.064 5 mg·g^-1, respectively. Except for manufacturer Q2, the contents of the products from the other manufacturers samples were maintained at (100±30)% of their respective average values, and the contents of the five components of manufacturer Q2 were mostly higher than 30% of the average value of all samples, indicating that there were great differences in product quality among different enterprises. The results of chemical pattern recognition showed that all samples could be roughly divided into two categories, indicating that the preparation process was relatively stable within the enterprise, but there were some differences between enterprises. The difference markers of the screened samples included the target components chlorogenic acid, hyperoside, and isochlorogenic acid B. CONCLUSION The quantitative method is accurate, rapid and feasible. Combined with chemical pattern recognition method, it can be used to evaluate the quality of DSZP.

Key words

Dashanzha pill / HPLC fingerprint / chemical pattern recognition / quality control / hyperoside / isochlorogenic acid B

引用本文

李运, 王苗, 刘晓玲, 许晓辉, 马海棠, 戚鹏飞, 邱国玉, 程显隆. 基于HPLC指纹图谱结合多成分含量测定和化学模式识别的大山楂丸质量评价. 中国药学杂志, 2024 , 59 (24) : 2372 -2383 . DOI: 10.11669/cpj.2024.24.010

Yun LI, Miao WANG, Xiaoling LIU, Xiaohui XU, Haitang MA, Pengfei QI, Guoyu QIU, Xian-long CHENG. Quality Evaluation of Dashanzha Pills Based on HPLC Fingerprint and Multi-Component Analysis Combined with Chemical Pattern Recognition[J]. Chinese Pharmaceutical Journal, 2024 , 59 (24) : 2372 -2383 . DOI: 10.11669/cpj.2024.24.010

正文

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作为我国中医药经典名方,大山楂丸(Dashanzha pills,DSZP)由山楂、六神曲(麸炒)、炒麦芽3味药细粉与炼蜜、水等混合而成的大蜜丸,具有消食化滞、调和脾胃的作用^[1]。“性味”是中药的特有属性,反映了中药的本质特征,是中药药性理论的核心。DSZP味酸,酸味能收能涩,该类药物的物质基础多以有机酸类为主。DSZP与复方消化酶对于肠胃消化功能的恢复均有促进作用,且相比于复方消化酶,DSZP具有价优质廉,安全性高的特点^[2]。山楂作为君药,又富含黄酮类成分,具有多种现代药理作用^[3-4]。在《中国药典》2020年版基础上,目前DSZP的质量控制多以单个成分的含量测定为主,且时间较久远^[5-6],缺乏系统性控制。当前药典中对DSZP的检测项目主要有性状、鉴别、检查、含量测定,从近年来国家药品评价抽检情况来看,中成药质量状况易受生产投料原料质量状、工艺等的影响,导致部分中成药出现一些质量问题^[7-9]。DSZP的安全性较好,受众人群广,需求量大,生产企业多,不同厂家、不同批次间的质量是否存在差异及整体质量如何尚无文献报道。故本文结合前期研究基础,基于中成药整体质量控制的理念,建立DSZP的指纹图谱,并对绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A等5种指标性成分进行含量测定,借助化学模式识别方法对多批次DSZP进行全面质量特征分析,旨在为其质量控制提供参考。

1 材料

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1.1 仪器

Waters e2695液相色谱仪(美国Waters 公司);调温型电热套(北京科伟永兴仪器有限公司);XSE205DU型电子天平(瑞士梅特勒-托利多公司);节能型智能恒温槽(宁波新芝生物科技股份有限公司);Centrifuge 5810R型离心机(艾本德公司);旋转蒸发仪(IKA公司)。

1.2 试剂

绿原酸(批号RDD-L00701908029,纯度98%,成都瑞芬思德丹生物科技有限公司);香草酸(批号:110722-201815,纯度:91.7%)、金丝桃苷(批号:111521-201809,纯度:94.9%)(中国食品药品检定研究院);异绿原酸A(批号:7867,纯度:98%)、异绿原酸B(批号:3089,纯度:98%)(上海诗丹德标准技术服务有限公司)。乙腈、甲醇均为色谱纯,纯化水为屈臣氏,其他试剂均为分析纯。

1.3 样品

DSZP均为市售样品,购自11个厂家51批次样品,样品来源信息见表1。

2 方法与结果

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2.1 溶液的制备

2.1.1 对照品溶液的制备

精密称取绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A等对照品适量,分别于10 mL量瓶中,甲醇溶解并定容,制得绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A质量浓度为1.025 1、1.074 7、0.918 6、1.010 4、0.973 1 mg·mL^-1的单一对照品溶液。精密吸取上述单一对照品溶液各适量,甲醇定容5 mL量瓶,得到绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A质量浓度分别为82.000 0、10.747 0、36.744 0、16.166 4、27.246 8 μg·mL^-1的混合对照品溶液,于4 ℃ 条件下保存,备用。

2.1.2 供试品溶液制备

取样品适量,剪碎,称取2 g,与硅藻土等比例混合后研成粉末。精密称定粉末2 g(精确至0.001 g),置于150 mL锥形瓶中,精密量取甲醇溶液25 mL,称量,加热回流提取1 h,静置放冷后再次称重,用甲醇溶液补足,离心(8 000 r·min^-1,5 min)后取出上清液,60 ℃减压浓缩,浓缩液转移至5 mL量瓶,甲醇少量多次冲洗,洗涤液一并转移至量瓶,甲醇定容至刻度,摇匀后0.45 μm有机微孔滤膜过滤,取续滤液即得。

2.1.3 阴性样品溶液制备

DSZP由山楂、麸炒六神曲、炒麦芽等3味药组方而成,《中国药典》2020年版收载DSZP项下制法为3种粉末直接与炼蜜等混合制成,故在阴性试验中与供试品溶液制备方法保持一致,分别制得山楂、麸炒六神曲、炒麦芽的单一样品溶液。

2.2 色谱条件

采用Agilent公司Eclipse Plus C₁₈色谱柱(4.6 mm×250 mm,5 μm);流动相:乙腈-0.1%甲酸水溶液,梯度洗脱:0~5 min,5%~6%乙腈;5~12 min,6%~12%乙腈;12~20 min,12%~15%乙腈;20~26 min,15%~19%乙腈;26~40 min,19%~33%乙腈;40~55 min,33%~55%乙腈;55~60 min,55%~75%乙腈;60~65 min,75%~90%乙腈;65~70 min,90%~5%乙腈70~72 min,5%乙腈;流速:1.0 mL·min^-1,检测波长:250 nm,柱温:30 ℃,进样量:10 μL。

2.3 指纹图谱研究

2.3.1 精密度试验

取DSZP(编号H4),按“2.1.2”项下方法进行供试品溶液的制备,按“2.2”项下色谱条件连续进样6次,以5号峰(绿原酸)为参照峰,测得各共有峰相对保留时间及相对峰面积的相对标准偏差(RSD)值,均小于3.0%,表明仪器精密度良好。

2.3.2 重复性试验

取DSZP(编号H4)平行6份,精密称定,按“2.1.2”项下方法制备供试品溶液,在“2.2”项下色谱条件进样测定,记录各色谱图。以5号峰(绿原酸)为参照峰,测得各共有峰相对保留时间及相对峰面积的RSD值,均小于3.0%,表明该方法重复性好。

2.3.3 稳定性试验

取DSZP(编号H4),按“2.1.2”项下方法制备供试品溶液,在“2.2”项色谱条件下,分别于0、2、4、8、12、24 h测定,记录各色谱图。以5号峰(绿原酸)为参照峰,测得各共有峰相对保留时间及相对峰面积的RSD值,均小于3.0%,表明供试品溶液于24 h内测定结果稳定。

2.3.4 对照指纹图谱的建立及相似度评价

取11个厂家产DSZP 51批样品,按“2.1.2”项下方法进行供试品溶液的制备,按“2.2”项下色谱条件采集色谱数据,对各色谱图进行积分后,导出AIA格式的文件,分别将其导入《中药色谱指纹图谱相似度评价系统(2012.130723 版本)》进行处理,将其他样品的色谱峰与参照图谱进行自动匹配,生成DSZP叠加图谱及对照图谱,见图1。设定H4为参照图谱,时间窗宽度设定为0.2 min,采用中位数法,进行全谱峰匹配,生成DSZP对照指纹图谱。共标定出16个共有峰,其中5号峰(绿原酸)稳定性好,色谱响应高,保留时间适中,故选择该色谱峰为参照峰(S),计算得51批DSZP指纹图谱相似度。结果表明,Q1~Q11 11个厂家生产DSZP的相似度分别为:0.919~1.000、0.829~0.958、0.920~0.980、0.653~0.676、0.872~0.982、0.866~0.889、0.709~0.839、0.713~0.740、0.641~0.647、0.633~0.636、0.657~0.671。

2.3.5 色谱峰归属及指认

精密吸取“2.1”项下各溶液,按“2.2”项下色谱条件进样分析,与指纹图谱共有峰进行对比。结果16个共有峰中的13个色谱峰分属于山楂、麸炒六神曲及炒麦芽,其余3个保留时间分别为7.97 min(2号峰)、34.71 min(11号峰)、58.24 min(13号峰)的色谱峰未能归属。

经与对照品比较指认了5个色谱峰,分别为绿原酸(5号峰)、香草酸(6号峰)、金丝桃苷(7号峰)、异绿原酸B(9号峰)、异绿原酸A(10号峰),见图2。

2.4 含量测定研究

2.4.1 专属性考察

取“2.1”项下3种溶液,在“2.2”色谱条件下进样,记录色谱图,目标成分均达到基线分离,可见供试品呈现与对照品保留时间一致的色谱峰。在阴性样品色谱图中,绿原酸、香草酸在3味药材中均可检测到,除此之外,山楂中可测到金丝桃苷和异绿原酸B,麸炒六神曲中可测到异绿原酸A和异绿原酸B,麦芽中可测到异绿原酸A,且炒麦芽和麸炒六神曲中整体色谱峰的响应值较低,具体见图3。

2.4.2 线性关系

分别吸取“2.1.1”项下混合对照品溶液0.1、0.2、0.4、0.8、1.2、1.6 mL,分别置于2 mL量瓶中,用甲醇定容至刻度,摇匀,配制成梯度浓度的混合对照品溶液,按照“2.2”项下色谱条件测定。以对照品溶液质量浓度(X,μg·mL^-1)为横坐标,峰面积(Y)为纵坐标进行标准曲线绘制,见表2。

2.4.3 方法学考察

按“2.1.2”项下方法制备供试品溶液,依“2.2”项下色谱条件,连续进样6次,结果绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A峰面积的RSD均<3%,表明仪器精密度良好。精密称取样品(编号:H4),按“2.1.2”项下方法平行制备6份溶液,按“2.2”项下色谱条件分别进样测定,绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A的平均含量分别为0.163 0、0.019 7、0.116 3、0.018 6、0.035 7 mg·g^-1,RSD均<3%,结果表明,该方法重复性良好。精密称取样品(编号:H4),按“2.1.2”项下方法制备供试品溶液,按“2.2”项下色谱条件,分别于0、2、4、8、12、24 h测定,结果绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A峰面积的RSD均<3%,结果表明,该方法在24 h内稳定性良好。

2.4.4 加样回收率试验

精密称取样品(编号:H4)0.5 g,平行6份,分别按1:1加入对照品溶液,在“2.1.2”项下方法制备供试品溶液,进样分析,计算回收率,结果绿原酸、香草酸、金丝桃苷、异绿原酸B、异绿原酸A平均加样回收率(n=6)分别为98.09%、107.15%、109.35%、96.27%、105.27%,RSD值均小于4.5%,结果见表3。

2.4.5 样品测定

对51 批大山楂丸按“2.1.2”项下方法制备供试品溶液,平行3份,在“2.2”项色谱条件进样分析,见表4。结果显示,所有样品中绿原酸的均值为0.133 0 mg·g^-1,香草酸均值为0.021 1 mg·g^-1,金丝桃苷均值为0.118 4 mg·g^-1,异绿原酸B均值为0.023 3 mg·g^-1,异绿原酸A均值为0.041 0 mg·g^-1,多个企业的目标化合物明显超出所有样品均值±30%,表明企业间的产品质量存在较大差异,单一投料药材对DSZP整体质量的影响有待进一步的深入研究;Q2企业中所有目标成分含量均不同程度超出所有样品均值±30%,为进一步突出含量差异,利用Origin 21制作含量雷达图,见图4。

3 化学模式识别研究

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3.1 聚类分析

对51批样品进行共有峰指认,得到16个共有峰,以绿原酸为参照峰,得到共有峰的相对保留时间,见表5。以此共有峰峰面积为原始数据,用SPSS 25进行聚类分析,具体见图5。可知,当组间距离为20时,所有样品可分为两类,Q1、Q3~Q13聚为一类,Q2单独聚为一类。表明被区分后的两类样品各自相似性较大,Q2与其余厂家样品的差异性显著。

3.2 主成分分析(PCA)

以51批样品的16个共有峰峰面积为变量进行最基本的降维分析(PCA), 导入 SPSS 25.0 软件,以特征值>1 为提取标准^[10],得到4个主成分因子,累积方差贡献率达到 75.709%,从一定程度上可为样本的质量评价提供参考依据。主成分及方差贡献率见表6。将共有成分峰面积导入 SIMCA 14.1 软件,经分析生成得分图,见图6,该结果与聚类分析结果基本一致。

3.3 正交偏最小二乘判别分析(OPLS-DA)

为进一步验证主成分分析结果的准确性,再次将共有成分峰面积导入SIMCA 14.1建立OPLS-DA模型,自动拟合后R²X、R²Y分别为0.940和0.603,预测能力参数Q²为0.536,OPLS-DA得分图见图7,同主成分分析结果一致。为防止过拟合现象出现,随后进行200次的置换检验,见图8,说明该模型稳定性较强,预测能力较好。变量重要性投影 (variable importance for the projection,VIP)是筛选不同样品间差异性化合物的重要指标,VIP 值越大,对差异的影响越大。经分析后得到16个共有成分的VIP值,结果见图9。以VIP值大于1为标准,得到8个变量,其中5号峰是绿原酸,7号峰是金丝桃苷,9号峰是异绿原酸B,即导致样品差异性的主要标志物。

4 讨论

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4.1 供试品溶液的制备方法考察

本研究对供试品溶液的提取方法(超声、回流)、提取时间(30 min、1 h)、提取溶剂为甲醇(体积分数30%、50%、70%、100%)、体积分数95%乙醇,提取体积(10、25、50 mL)进行了系统考察。综合考虑样品的提取率、整体色谱行为、色谱峰信息的丰富情况、主要色谱峰的峰形、分离度及峰面积,环境的友好性。最终确定,当2 g样品中加入25 mL的甲醇,加热回流提取1 h为最佳提取条件。

4.2 指纹图谱及含量测定化学模式识别结果

本实验首次建立了11个生产厂家51批 DSZP的指纹图谱,能够较全面地对市售DSZP 的质量状况进行评估。整体样本指纹图谱的相似度介于0.633~1.000,其中Q1、Q3两厂家产品相似度均大于0.9,接近1.0;Q2、Q5、Q6三个厂家产品相似度均大于0.8,接近0.9;Q4、Q9、Q10、Q11四个厂家产品相似度均在0.65左右,由此提示,同一厂家产品间一致性较好,不同厂家产品间存在较大差异。基于指纹图谱的构建,可以弥补中成药质量控制指标与临床关系不紧密、“碎片化”的现象。探索中成药产品质量一致性的评价策略^[11-12],保障临床用药的安全、有效,意义重大。DSZP中指标性成分定量测定结果表明,同一厂家产DSZP中指标性成分的含量基本保持在各自均值的±30%,说明不同企业内部不同批号样品的均一性较好,生产工艺环境稳定可靠。在此基础上,厂家Q2的5种指标性成分含量显著高于所有样品均值的±30%,加之16个共有峰峰面积整体偏大,表明Q2厂家DSZP的整体质量要优于其余厂家样品,也表明不同企业间的产品质量存在较大差异,初步推测受投料原料质量状况影响较大。通过化学模式识别的方法进行更进一步的数据挖掘,聚类分析表明,当欧式距离为15时,所有样品大致可分为3类,当欧式距离为20时,样品可被聚为两类,其中Q2始终被单独聚为一类。由主成分分析得分图可知,该分析结果与聚类结果保持一致,OPLS-DA中筛选得到8个影响样品间差异性原因的变量因子,其中包含定量分析的绿原酸、金丝桃苷和异绿原酸B。这3个目标成分主要存在于山楂中,大山楂丸中规定山楂以生品入药,但不排除某些企业用其他炮制品代替,Luo等^[13]研究山楂炒焦前后DSZP化学成分进行分析,发现生品与焦品存在部分共有成分,其中包含绿原酸。因此,企业在生产前应严格把控投料药材的质量。

5 分析与总结

收起

《中国药典》2020年版收载DSZP【鉴别】项下,对山楂、炒麦芽的部分显微特征进行了描述;通过盐酸-镁粉反应对黄酮类化合物进行了鉴别;利用TLC法对熊果酸进行鉴别。【含量测定】项下,采用薄层扫描法,建立了熊果酸的含量测定方法,仅对投料山楂的质量进行控制。由此可见,对于DSZP的质量控制手段较为单一,未能有效对投料进行全面的控制,难以反映其整体内在质量。同时,处方中六神曲的制法收载于《卫生部药品标准·中药成方制剂》^[14]《全国中药炮制规范》^[15],但全国各省地方标准亦多有收载^[16-19],受发酵环境、终点确定等的影响,致使六神曲的品质良莠不齐,这可能是导致DSZP质量差异的重要原因,值得进一步关注。中成药通常由多味中药组方而成,物质组成复杂、多样,是其发挥药效的关键,同时也是全面的质量控制的难点。指纹图谱技术可以整体地展示被测样品的化学特征全貌,是最适合中成药整体质量控制的技术之一^[20],结合多指标成分定量测定,运用化学模式识别对测定数据进行深度挖掘表征,可进一步提升质量控制水平。

本试验建立了一种DSZP中HPLC法同时测定多成分含量方法,并结合化学计量学统计分析方法对51批样品整体进行质量评价。该方法结果可靠,准确性高,能够反映出市售DSZP的质量情况,可为山楂丸的质量标准提升提供参考。

基金

收起

甘肃省药品科研项目(2022GSMPA0037)
陇原青年创新创业人才项目(2023LQGR49)
兰州市青年科技人才创新项目(2023-QN-144)
兰州市科技计划项目(2022-2-2)

参考文献

收起

文献

收起

参考文献引证文献

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2024年第59卷第24期

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文章信息

doi: 10.11669/cpj.2024.24.010

接收时间：2024-07-08
首发时间：2025-11-13
出版时间：2024-12-22

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文章信息

作者

出版历史

收稿日期：2024-07-08

基金

甘肃省药品科研项目(2022GSMPA0037)

陇原青年创新创业人才项目(2023LQGR49)

兰州市青年科技人才创新项目(2023-QN-144)

兰州市科技计划项目(2022-2-2)

作者信息

¹ 兰州市食品药品检验检测研究院, 兰州 730050

² 甘肃中医药大学药学院, 兰州 730000

³ 甘肃药业集团科技创新研究院有限公司, 兰州 730000

⁴ 中国食品药品检定研究院, 北京 100050

通讯作者:

^* 程显隆,男,研究员研究方向:中药质量控制研究 Tel:(010)67095432

参考文献

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

关闭全屏

BibTeX
EndNote
RefWorks
TxT

No.	Enterprise	Batch number number	Source(in Chinese)	No.	Enterprise	Batch number	Source(in Chinese)
H1	Q1	19015202	Lanzhou(兰州)	H27	Q5	20221223	Tianjin(天津)
H2		22015043	Xingtai(邢台)	H28		20230226	Changchun(长春)
H3		22015056	Beijing(北京)	H29		20230334	Shanghai(上海)
H4		22015090	Xi'an(西安)	H30		20230343	Shijiazhuang(石家庄)
H5		22015091	Xingtai(邢台)	H31		20230501	Jinan(济南)
H6		21015100	Chengdu(成都)	H32		20230504	Yichun(宜春)
H7		22015148	Taiyuan(太原)	H33		20230507	Haerbin(哈尔滨)
H8		22015149	Luohe(洛阳)	H34	Q6	121010	Tianjin(天津)
H9		22015150	Zhengzhou(郑州)	H35		122003	Shuozhou(朔州)
H10		22015151	Beijing(北京)	H36		123002	Taiyuan(太原)
H11		21015187	Chongqing(重庆)	H37	Q7	2220305	Fuyang(阜阳)
H12		21015395	Qingdao(青岛)	H38		2220305	Fuyang(阜阳)
H13	Q2	131065	Jinan(济南)	H39		2220902	Beijing(北京)
H14		131065	Changsha(长沙)	H40	Q8	20210680	Mianyang(绵阳)
H15		131069	Fuyang(阜阳)	H41		20210680	Zhengzhou(郑州)
H16		131069	Heze(菏泽)	H42		20220102	Changzhi(长治)
H17		131069	Yichun(宜春)	H43	Q9	220401	Zhengzhou(郑州)
H18		131070	Dezhou(德州)	H44		230501	Zhengzhou(郑州)
H19	Q3	210401	Changchun(长春)	H45		230501	Kaifeng(开封)
H20		211201	Handan(邯郸)	H46	Q10	WJ21056	Haerbin(哈尔滨)
H21		220701	Anshan(鞍山)	H47		WJ21057	Zhengzhou(郑州)
H22		220701	Yichun(宜春)	H48		WJ22115	Chengdu(成都)
H23	Q4	20220572	Chaoyang(朝阳)	H49	Q11	20211217	Kunming(昆明)
H24		20221221	Hengyang(衡阳)	H50		20230638	Shaoguan(韶关)
H25		20230411	Guangzhou(广州)	H51		20230638	Shaoguan(韶关)
H26		20230412	Wuhan(武汉)

No.

Enterprise

Batch number number

Source(in Chinese)

No.

Enterprise

Batch number

Source(in Chinese)

19015202

Lanzhou(兰州)

H27

20221223

Tianjin(天津)

22015043

Xingtai(邢台)

H28

20230226

Changchun(长春)

22015056

Beijing(北京)

H29

20230334

Shanghai(上海)

22015090

Xi'an(西安)

H30

20230343

Shijiazhuang(石家庄)

22015091

Xingtai(邢台)

H31

20230501

Jinan(济南)

21015100

Chengdu(成都)

H32

20230504

Yichun(宜春)

22015148

Taiyuan(太原)

H33

20230507

Haerbin(哈尔滨)

22015149

Luohe(洛阳)

H34

121010

Tianjin(天津)

22015150

Zhengzhou(郑州)

H35

122003

Shuozhou(朔州)

H10

22015151

Beijing(北京)

H36

123002

Taiyuan(太原)

H11

21015187

Chongqing(重庆)

H37

2220305

Fuyang(阜阳)

H12

21015395

Qingdao(青岛)

H38

2220305

Fuyang(阜阳)

H13

131065

Jinan(济南)

H39

2220902

Beijing(北京)

H14

131065

Changsha(长沙)

H40

20210680

Mianyang(绵阳)

H15

131069

Fuyang(阜阳)

H41

20210680

Zhengzhou(郑州)

H16

131069

Heze(菏泽)

H42

20220102

Changzhi(长治)

H17

131069

Yichun(宜春)

H43

220401

Zhengzhou(郑州)

H18

131070

Dezhou(德州)

H44

230501

Zhengzhou(郑州)

H19

210401

Changchun(长春)

H45

230501

Kaifeng(开封)

H20

211201

Handan(邯郸)

H46

Q10

WJ21056

Haerbin(哈尔滨)

H21

220701

Anshan(鞍山)

H47

WJ21057

Zhengzhou(郑州)

H22

220701

Yichun(宜春)

H48

WJ22115

Chengdu(成都)

H23

20220572

Chaoyang(朝阳)

H49

Q11

20211217

Kunming(昆明)

H24

20221221

Hengyang(衡阳)

H50

20230638

Shaoguan(韶关)

H25

20230411

Guangzhou(广州)

H51

20230638

Shaoguan(韶关)

H26

20230412

Wuhan(武汉)

Componnet	Regression equation	Linearity range/μg·mL^-1	r
Chlorogenic acid	Y=1.21×10⁴X-2.35×10⁴	4.10	-65.60	0.998 9
Vanillic acid	Y=2.15×10⁴X-1.98×10³	0.54	-8.60	0.998 0
Hyperoside	Y=8.47×10³X-2.87×10³	1.84	-29.40	0.999 0
Isochlorogenic acid B	Y=1.43×10⁴X-2.78×10³	0.81	-12.93	0.998 9
Isochlorogenic acid A	Y=1.62×10⁴X-8.87×10³	1.36	-21.80	0.999 1

Componnet

Regression equation

Linearity range/μg·mL^-1

Chlorogenic acid

Y=1.21×10⁴X-2.35×10⁴

4.10

-65.60

0.998 9

Vanillic acid

Y=2.15×10⁴X-1.98×10³

0.54

-8.60

0.998 0

Hyperoside

Y=8.47×10³X-2.87×10³

1.84

-29.40

0.999 0

Isochlorogenic acid B

Y=1.43×10⁴X-2.78×10³

0.81

-12.93

0.998 9

Isochlorogenic acid A

Y=1.62×10⁴X-8.87×10³

1.36

-21.80

0.999 1

Componnet	m(Original)/μg	m(Sample)/g	m(Added)/μg	m(Measured)/μg	Recovery/%	Average recovery/%	RSD/%
Chlorogenic acid	81.822 2	0.502 0	82.000 0	157.011 9	91.69	98.09	4.07
	82.474 2	0.506 0	82.000 0	162.548 3	97.65
	81.659 2	0.501 0	82.000 0	160.455 4	96.09
	82.148 2	0.504 0	82.000 0	163.511 8	99.22
	81.903 7	0.502 5	82.000 0	166.584 9	103.27
	81.985 2	0.503 0	82.000 0	164.485 6	100.61
Vanillic acid	9.866 9	0.502 0	9.672 3	20.334 6	108.22	107.15	3.69
	9.945 5	0.506 0	9.672 3	20.425 0	108.35
	9.847 2	0.501 0	9.672 3	20.126 3	106.27
	9.906 2	0.504 0	9.672 3	20.575 9	110.31
	9.876 7	0.502 5	9.672 3	20.524 5	110.08
	9.886 5	0.503 0	9.672 3	19.524 2	99.64
Hyperoside	58.402 9	0.502 0	57.871 8	122.516 4	110.79	109.35	3.65
	58.868 2	0.506 0	57.871 8	118.429 6	102.92
	58.286 5	0.501 0	57.871 8	124.197 1	113.89
	58.635 5	0.504 0	57.871 8	120.332 2	106.61
	58.461 0	0.502 5	57.871 8	121.960 2	109.72
	58.519 2	0.503 0	57.871 8	123.426 4	112.16
Isochlorogenic acid B	9.323 1	0.502 0	9.382 5	18.202 4	94.64	96.27	3.92
	9.397 3	0.506 0	9.382 5	18.978 0	102.11
	9.304 5	0.501 0	9.382 5	18.338 6	96.29
	9.360 2	0.504 0	9.382 5	17.867 5	90.67
	9.332 3	0.502 5	9.382 5	18.528 1	98.01
	9.341 6	0.503 0	9.382 5	18.337 8	95.88
Isochlorogenic acid A	17.902 5	0.502 0	17.351 5	36.739 2	108.56	105.27	2.83
	18.045 1	0.506 0	17.351 5	35.629 9	101.34
	17.866 8	0.501 0	17.351 5	36.405 2	106.84
	17.973 8	0.504 0	17.351 5	36.718 2	108.03
	17.920 3	0.502 5	17.351 5	35.735 6	102.67
	17.938 2	0.503 0	17.351 5	36.010 0	104.15

Componnet

m(Original)/μg

m(Sample)/g

m(Added)/μg

m(Measured)/μg

Recovery/%

Average recovery/%

RSD/%

Chlorogenic acid

81.822 2

0.502 0

82.000 0

157.011 9

91.69

98.09

4.07

82.474 2

0.506 0

82.000 0

162.548 3

97.65

81.659 2

0.501 0

82.000 0

160.455 4

96.09

82.148 2

0.504 0

82.000 0

163.511 8

99.22

81.903 7

0.502 5

82.000 0

166.584 9

103.27

81.985 2

0.503 0

82.000 0

164.485 6

100.61

Vanillic acid

9.866 9

0.502 0

9.672 3

20.334 6

108.22

107.15

3.69

9.945 5

0.506 0

9.672 3

20.425 0

108.35

9.847 2

0.501 0

9.672 3

20.126 3

106.27

9.906 2

0.504 0

9.672 3

20.575 9

110.31

9.876 7

0.502 5

9.672 3

20.524 5

110.08

9.886 5

0.503 0

9.672 3

19.524 2

99.64

Hyperoside

58.402 9

0.502 0

57.871 8

122.516 4

110.79

109.35

3.65

58.868 2

0.506 0

57.871 8

118.429 6

102.92

58.286 5

0.501 0

57.871 8

124.197 1

113.89

58.635 5

0.504 0

57.871 8

120.332 2

106.61

58.461 0

0.502 5

57.871 8

121.960 2

109.72

58.519 2

0.503 0

57.871 8

123.426 4

112.16

Isochlorogenic acid B

9.323 1

0.502 0

9.382 5

18.202 4

94.64

96.27

3.92

9.397 3

0.506 0

9.382 5

18.978 0

102.11

9.304 5

0.501 0

9.382 5

18.338 6

96.29

9.360 2

0.504 0

9.382 5

17.867 5

90.67

9.332 3

0.502 5

9.382 5

18.528 1

98.01

9.341 6

0.503 0

9.382 5

18.337 8

95.88

Isochlorogenic acid A

17.902 5

0.502 0

17.351 5

36.739 2

108.56

105.27

2.83

18.045 1

0.506 0

17.351 5

35.629 9

101.34

17.866 8

0.501 0

17.351 5

36.405 2

106.84

17.973 8

0.504 0

17.351 5

36.718 2

108.03

17.920 3

0.502 5

17.351 5

35.735 6

102.67

17.938 2

0.503 0

17.351 5

36.010 0

104.15

No.	Chlorogenic acid	Vanillic acid	Hyperoside	Isochlorogenic acid B	Isochlorogenic acid A	No.	Chlorogenic acid	Vanillic acid	Hyperos ide	Isochlorogenic acid B	Isochlorogenic acid A
H1	0.104 2	0.024 1	0.097 6	0.020 5	0.039 7	H27	0.147 1	0.019 2	0.127 3	0.031 5	0.053 8
H2	0.153 4	0.021 7	0.145 7	0.035 0	0.047 5	H28	0.199 2	0.023 0	0.120 8	0.026 0	0.046 4
H3	0.156 0	0.023 4	0.129 5	0.026 9	0.043 1	H29	0.205 9	0.028 2	0.146 8	0.039 7	0.055 0
H4	0.152 2	0.021 7	0.121 1	0.021 5	0.032 9	H30	0.193 6	0.036 2	0.162 4	0.027 1	0.045 8
H5	0.154 1	0.021 7	0.118 7	0.025 7	0.044 3	H31	0.205 6	0.031 9	0.174 1	0.041 4	0.058 3
H6	0.094 5	0.018 6	0.078 7	0.013 3	0.028 9	H32	0.178 2	0.022 1	0.132 6	0.027 3	0.042 4
H7	0.148 0	0.023 4	0.134 7	0.023 9	0.038 2	H33	0.206 0	0.034 6	0.163 4	0.021 7	0.040 1
H8	0.149 1	0.022 7	0.145 2	0.039 3	0.044 6	H34	0.085 8	0.016 5	0.113 4	0.021 4	0.030 1
H9	0.148 6	0.021 7	0.133 9	0.036 7	0.050 6	H35	0.088 1	0.014 9	0.106 3	0.020 6	0.026 0
H10	0.154 4	0.023 1	0.139 0	0.026 4	0.038 3	H36	0.173 8	0.029 0	0.133 5	0.020 2	0.033 2
H11	0.118 2	0.016 7	0.100 8	0.014 8	0.027 4	H37	0.129 7	0.019 6	0.078 3	0.014 6	0.047 3
H12	0.184 1	0.023 7	0.113 6	0.025 1	0.043 0	H38	0.130 0	0.019 2	0.085 2	0.026 4	0.064 5
H13	0.227 0	0.023 2	0.226 1	0.034 3	0.021 7	H39	0.053 6	0.014 5	0.098 7	0.017 6	0.046 4
H14	0.189 4	0.019 2	0.214 4	0.032 9	0.022 4	H40	0.122 8	0.011 7	0.060 1	0.015 6	0.034 1
H15	0.205 9	0.031 0	0.370 2	0.063 2	0.037 1	H41	0.118 9	0.012 2	0.056 9	0.013 3	0.027 2
H16	0.200 8	0.021 3	0.353 9	0.057 0	0.029 3	H42	0.097 1	0.009 7	0.097 5	0.018 1	0.026 7
H17	0.192 6	0.021 9	0.341 4	0.057 6	0.037 9	H43	0.093 3	0.013 3	0.023 0	0.006 6	0.041 4
H18	0.206 9	0.031 4	0.363 6	0.057 3	0.033 0	H44	0.081 0	0.012 1	0.028 9	0.009 6	0.042 1
H19	0.135 2	0.016 9	0.110 7	0.017 8	0.035 9	H45	0.084 7	0.015 5	0.032 7	0.011 1	0.043 8
H20	0.121 9	0.021 0	0.109 7	0.020 7	0.037 6	H46	0.077 5	0.018 3	0.031 2	0.017 9	0.056 8
H21	0.135 7	0.021 3	0.104 9	0.026 4	0.045 3	H47	0.067 9	0.016 8	0.032 3	0.016 6	0.047 1
H22	0.131 4	0.021 5	0.088 9	0.020 2	0.040 0	H48	0.063 5	0.019 6	0.036 7	0.014 8	0.056 4
H23	0.133 5	0.022 7	0.026 2	0.009 6	0.042 4	H49	0.053 8	0.018 0	0.036 4	0.009 1	0.043 5
H24	0.117 2	0.023 9	0.027 8	0.010 5	0.041 5	H50	0.047 2	0.016 9	0.035 5	0.006 4	0.053 8
H25	0.116 9	0.018 8	0.038 0	0.010 8	0.049 8	H51	0.056 4	0.018 4	0.034 0	0.006 5	0.053 0
H26	0.118 0	0.018 1	0.042 1	0.008 7	0.043 1

No.

Chlorogenic
acid

Vanillic
acid

Hyperoside

Isochlorogenic
acid B

Isochlorogenic
acid A

No.

Chlorogenic
acid

Vanillic
acid

Hyperos
ide

Isochlorogenic
acid B

Isochlorogenic
acid A

0.104 2

0.024 1

0.097 6

0.020 5

0.039 7

H27

0.147 1

0.019 2

0.127 3

0.031 5

0.053 8

0.153 4

0.021 7

0.145 7

0.035 0

0.047 5

H28

0.199 2

0.023 0

0.120 8

0.026 0

0.046 4

0.156 0

0.023 4

0.129 5

0.026 9

0.043 1

H29

0.205 9

0.028 2

0.146 8

0.039 7

0.055 0

0.152 2

0.021 7

0.121 1

0.021 5

0.032 9

H30

0.193 6

0.036 2

0.162 4

0.027 1

0.045 8

0.154 1

0.021 7

0.118 7

0.025 7

0.044 3

H31

0.205 6

0.031 9

0.174 1

0.041 4

0.058 3

0.094 5

0.018 6

0.078 7

0.013 3

0.028 9

H32

0.178 2

0.022 1

0.132 6

0.027 3

0.042 4

0.148 0

0.023 4

0.134 7

0.023 9

0.038 2

H33

0.206 0

0.034 6

0.163 4

0.021 7

0.040 1

0.149 1

0.022 7

0.145 2

0.039 3

0.044 6

H34

0.085 8

0.016 5

0.113 4

0.021 4

0.030 1

0.148 6

0.021 7

0.133 9

0.036 7

0.050 6

H35

0.088 1

0.014 9

0.106 3

0.020 6

0.026 0

H10

0.154 4

0.023 1

0.139 0

0.026 4

0.038 3

H36

0.173 8

0.029 0

0.133 5

0.020 2

0.033 2

H11

0.118 2

0.016 7

0.100 8

0.014 8

0.027 4

H37

0.129 7

0.019 6

0.078 3

0.014 6

0.047 3

H12

0.184 1

0.023 7

0.113 6

0.025 1

0.043 0

H38

0.130 0

0.019 2

0.085 2

0.026 4

0.064 5

H13

0.227 0

0.023 2

0.226 1

0.034 3

0.021 7

H39

0.053 6

0.014 5

0.098 7

0.017 6

0.046 4

H14

0.189 4

0.019 2

0.214 4

0.032 9

0.022 4

H40

0.122 8

0.011 7

0.060 1

0.015 6

0.034 1

H15

0.205 9

0.031 0

0.370 2

0.063 2

0.037 1

H41

0.118 9

0.012 2

0.056 9

0.013 3

0.027 2

H16

0.200 8

0.021 3

0.353 9

0.057 0

0.029 3

H42

0.097 1

0.009 7

0.097 5

0.018 1

0.026 7

H17

0.192 6

0.021 9

0.341 4

0.057 6

0.037 9

H43

0.093 3

0.013 3

0.023 0

0.006 6

0.041 4

H18

0.206 9

0.031 4

0.363 6

0.057 3

0.033 0

H44

0.081 0

0.012 1

0.028 9

0.009 6

0.042 1

H19

0.135 2

0.016 9

0.110 7

0.017 8

0.035 9

H45

0.084 7

0.015 5

0.032 7

0.011 1

0.043 8

H20

0.121 9

0.021 0

0.109 7

0.020 7

0.037 6

H46

0.077 5

0.018 3

0.031 2

0.017 9

0.056 8

H21

0.135 7

0.021 3

0.104 9

0.026 4

0.045 3

H47

0.067 9

0.016 8

0.032 3

0.016 6

0.047 1

H22

0.131 4

0.021 5

0.088 9

0.020 2

0.040 0

H48

0.063 5

0.019 6

0.036 7

0.014 8

0.056 4

H23

0.133 5

0.022 7

0.026 2

0.009 6

0.042 4

H49

0.053 8

0.018 0

0.036 4

0.009 1

0.043 5

H24

0.117 2

0.023 9

0.027 8

0.010 5

0.041 5

H50

0.047 2

0.016 9

0.035 5

0.006 4

0.053 8

H25

0.116 9

0.018 8

0.038 0

0.010 8

0.049 8

H51

0.056 4

0.018 4

0.034 0

0.006 5

0.053 0

H26

0.118 0

0.018 1

0.042 1

0.008 7

0.043 1

Batch No.	t1	t2	t3	t4	t5	t6	t7	t8	t9	t10	t11	t12	t13	t14	t15	t16
H1	0.394	0.472	0.647	0.715	1.000	1.101	1.846	1.876	1.977	2.035	2.072	2.605	3.454	3.766	3.842	3.904
H2	0.393	0.474	0.650	0.719	1.000	1.100	1.828	1.858	1.958	2.016	2.053	2.580	3.424	3.734	3.809	3.871
H3	0.394	0.473	0.649	0.714	1.000	1.100	1.838	1.868	1.969	2.027	2.065	2.597	3.452	3.767	3.843	3.906
H4	0.392	0.471	0.648	0.716	1.000	1.101	1.834	1.865	1.966	2.025	2.062	2.596	3.452	3.767	3.843	3.905
H5	0.391	0.472	0.648	0.716	1.000	1.100	1.832	1.863	1.963	2.023	2.060	2.594	3.450	3.764	3.840	3.904
H6	0.391	0.472	0.649	0.716	1.000	1.100	1.832	1.864	1.965	2.025	2.063	2.595	3.452	3.767	3.844	3.906
H7	0.391	0.471	0.648	0.716	1.000	1.100	1.831	1.861	1.962	2.023	2.060	2.592	3.445	3.758	3.834	3.898
H8	0.393	0.472	0.650	0.716	1.000	1.100	1.835	1.866	1.969	2.027	2.065	2.596	3.451	3.765	3.841	3.904
H9	0.394	0.473	0.650	0.719	1.000	1.101	1.831	1.861	1.962	2.021	2.059	2.589	3.443	3.757	3.833	3.898
H10	0.389	0.467	0.647	0.714	1.000	1.101	1.834	1.864	1.966	2.026	2.064	2.599	3.454	3.771	3.847	3.912
H11	0.385	0.469	0.647	0.715	1.000	1.102	1.838	1.869	1.973	2.032	2.070	2.610	3.467	3.784	3.861	3.925
H12	0.389	0.469	0.647	0.714	1.000	1.101	1.833	1.863	1.965	2.024	2.062	2.594	3.447	3.759	3.836	3.899
H13	0.386	0.466	0.649	0.713	1.000	1.101	1.844	1.875	1.979	2.038	2.078	2.620	3.486	3.804	3.882	3.946
H14	0.386	0.469	0.648	0.711	1.000	1.102	1.849	1.880	1.985	2.044	2.082	2.622	3.482	3.800	3.879	3.942
H15	0.386	0.466	0.649	0.713	1.000	1.101	1.842	1.873	1.978	2.039	2.077	2.616	3.484	3.798	3.877	3.940
H16	0.389	0.463	0.647	0.714	1.000	1.101	1.836	1.867	1.970	2.028	2.066	2.602	3.458	3.774	3.851	3.914
H17	0.391	0.468	0.648	0.714	1.000	1.102	1.838	1.870	1.974	2.035	2.071	2.611	3.474	3.789	3.868	3.931
H18	0.398	0.473	0.662	0.732	1.000	1.121	1.863	1.894	1.998	2.057	2.096	2.636	3.500	3.818	3.897	3.962
H19	0.389	0.472	0.648	0.716	1.000	1.099	1.826	1.856	1.959	2.019	2.056	2.588	3.445	3.762	3.838	3.899
H20	0.393	0.475	0.654	0.720	1.000	1.104	1.839	1.870	1.972	2.032	2.070	2.600	3.458	3.775	3.852	3.914
H21	0.395	0.476	0.653	0.719	1.000	1.103	1.841	1.872	1.975	2.034	2.071	2.608	3.468	3.787	3.864	3.926
H22	0.388	0.473	0.651	0.717	1.000	1.103	1.834	1.864	1.968	2.027	2.064	2.597	3.456	3.775	3.851	3.914
H23	0.390	0.474	0.653	0.719	1.000	1.102	1.834	1.865	1.964	2.025	2.064	2.598	3.453	3.772	3.849	3.912
H24	0.391	0.474	0.652	0.718	1.000	1.103	1.832	1.864	1.967	2.025	2.062	2.596	3.452	3.770	3.846	3.909
H25	0.390	0.474	0.654	0.720	1.000	1.102	1.827	1.857	1.961	2.019	2.058	2.588	3.441	3.757	3.834	3.898
H26	0.390	0.474	0.654	0.721	1.000	1.103	1.832	1.863	1.962	2.023	2.060	2.594	3.452	3.769	3.846	3.908
H27	0.391	0.475	0.653	0.717	1.000	1.103	1.830	1.861	1.964	2.025	2.063	2.600	3.463	3.791	3.867	3.927
H28	0.390	0.475	0.653	0.716	1.000	1.103	1.833	1.864	1.968	2.029	2.067	2.604	3.469	3.798	3.874	3.936
H29	0.389	0.474	0.654	0.718	1.000	1.101	1.832	1.863	1.969	2.029	2.067	2.607	3.471	3.802	3.879	3.942
H30	0.390	0.474	0.654	0.718	1.000	1.101	1.834	1.865	1.970	2.031	2.069	2.607	3.472	3.803	3.880	3.943
H31	0.389	0.474	0.652	0.717	1.000	1.101	1.831	1.862	1.965	2.026	2.064	2.599	3.459	3.788	3.863	3.923
H32	0.389	0.473	0.650	0.716	1.000	1.101	1.831	1.862	1.965	2.026	2.064	2.599	3.461	3.790	3.867	3.930
H33	0.389	0.474	0.653	0.719	1.000	1.101	1.829	1.860	1.962	2.023	2.061	2.593	3.451	3.778	3.853	3.915
H34	0.389	0.474	0.652	0.713	1.000	1.103	1.835	1.866	1.969	2.031	2.068	2.603	3.464	3.794	3.870	3.932
H35	0.385	0.470	0.648	0.712	1.000	1.097	1.826	1.859	1.966	2.025	2.063	2.603	3.471	3.802	3.877	3.937
H36	0.388	0.471	0.652	0.716	1.000	1.103	1.830	1.862	1.966	2.027	2.065	2.604	3.470	3.801	3.876	3.938
H37	0.384	0.469	0.651	0.714	1.000	1.103	1.834	1.866	1.971	2.032	2.070	2.607	3.474	3.804	3.879	3.942
H38	0.392	0.475	0.655	0.718	1.000	1.104	1.830	1.861	1.964	2.025	2.063	2.597	3.456	3.785	3.860	3.921
H39	0.389	0.475	0.655	0.720	1.000	1.104	1.830	1.861	1.966	2.025	2.063	2.596	3.456	3.784	3.858	3.919
H40	0.391	0.475	0.656	0.719	1.000	1.103	1.828	1.859	1.962	2.023	2.060	2.593	3.451	3.776	3.852	3.914
H41	0.389	0.474	0.655	0.718	1.000	1.105	1.831	1.863	1.947	2.028	2.066	2.601	3.460	3.788	3.862	3.925
H42	0.390	0.474	0.654	0.719	1.000	1.103	1.828	1.860	1.963	2.023	2.060	2.593	3.449	3.776	3.852	3.911
H43	0.385	0.473	0.661	0.717	1.000	1.104	1.834	1.866	1.972	2.029	2.069	2.605	3.469	3.799	3.875	3.936
H44	0.388	0.474	0.661	0.718	1.000	1.104	1.831	1.862	1.973	2.028	2.066	2.602	3.464	3.792	3.870	3.930
H45	0.386	0.473	0.653	0.718	1.000	1.102	1.831	1.863	1.971	2.027	2.066	2.605	3.467	3.798	3.873	3.938
H46	0.385	0.472	0.652	0.715	1.000	1.102	1.835	1.867	1.971	2.030	2.069	2.604	3.463	3.795	3.870	3.934
H47	0.386	0.472	0.652	0.714	1.000	1.102	1.833	1.864	1.970	2.027	2.066	2.599	3.462	3.791	3.866	3.931
H48	0.385	0.472	0.652	0.717	1.000	1.102	1.835	1.866	1.973	2.028	2.068	2.603	3.464	3.792	3.867	3.933
H49	0.383	0.472	0.652	0.716	1.000	1.103	1.830	1.863	1.970	2.026	2.066	2.602	3.463	3.793	3.867	3.933
H50	0.385	0.472	0.651	0.716	1.000	1.101	1.831	1.863	1.966	2.024	2.064	2.599	3.461	3.790	3.865	3.930
H51	0.383	0.471	0.651	0.717	1.000	1.102	1.826	1.858	1.961	2.020	2.061	2.596	3.455	3.784	3.859	3.923
RSD/%	0.831	0.581	0.548	0.436	0.000	0.284	0.342	0.336	0.375	0.328	0.331	0.354	0.370	0.438	0.434	0.430

Batch No.

t10

t11

t12

t13

t14

t15

t16

0.394

0.472

0.647

0.715

1.000

1.101

1.846

1.876

1.977

2.035

2.072

2.605

3.454

3.766

3.842

3.904

0.393

0.474

0.650

0.719

1.000

1.100

1.828

1.858

1.958

2.016

2.053

2.580

3.424

3.734

3.809

3.871

0.394

0.473

0.649

0.714

1.000

1.100

1.838

1.868

1.969

2.027

2.065

2.597

3.452

3.767

3.843

3.906

0.392

0.471

0.648

0.716

1.000

1.101

1.834

1.865

1.966

2.025

2.062

2.596

3.452

3.767

3.843

3.905

0.391

0.472

0.648

0.716

1.000

1.100

1.832

1.863

1.963

2.023

2.060

2.594

3.450

3.764

3.840

3.904

0.391

0.472

0.649

0.716

1.000

1.100

1.832

1.864

1.965

2.025

2.063

2.595

3.452

3.767

3.844

3.906

0.391

0.471

0.648

0.716

1.000

1.100

1.831

1.861

1.962

2.023

2.060

2.592

3.445

3.758

3.834

3.898

0.393

0.472

0.650

0.716

1.000

1.100

1.835

1.866

1.969

2.027

2.065

2.596

3.451

3.765

3.841

3.904

0.394

0.473

0.650

0.719

1.000

1.101

1.831

1.861

1.962

2.021

2.059

2.589

3.443

3.757

3.833

3.898

H10

0.389

0.467

0.647

0.714

1.000

1.101

1.834

1.864

1.966

2.026

2.064

2.599

3.454

3.771

3.847

3.912

H11

0.385

0.469

0.647

0.715

1.000

1.102

1.838

1.869

1.973

2.032

2.070

2.610

3.467

3.784

3.861

3.925

H12

0.389

0.469

0.647

0.714

1.000

1.101

1.833

1.863

1.965

2.024

2.062

2.594

3.447

3.759

3.836

3.899

H13

0.386

0.466

0.649

0.713

1.000

1.101

1.844

1.875

1.979

2.038

2.078

2.620

3.486

3.804

3.882

3.946

H14

0.386

0.469

0.648

0.711

1.000

1.102

1.849

1.880

1.985

2.044

2.082

2.622

3.482

3.800

3.879

3.942

H15

0.386

0.466

0.649

0.713

1.000

1.101

1.842

1.873

1.978

2.039

2.077

2.616

3.484

3.798

3.877

3.940

H16

0.389

0.463

0.647

0.714

1.000

1.101

1.836

1.867

1.970

2.028

2.066

2.602

3.458

3.774

3.851

3.914

H17

0.391

0.468

0.648

0.714

1.000

1.102

1.838

1.870

1.974

2.035

2.071

2.611

3.474

3.789

3.868

3.931

H18

0.398

0.473

0.662

0.732

1.000

1.121

1.863

1.894

1.998

2.057

2.096

2.636

3.500

3.818

3.897

3.962

H19

0.389

0.472

0.648

0.716

1.000

1.099

1.826

1.856

1.959

2.019

2.056

2.588

3.445

3.762

3.838

3.899

H20

0.393

0.475

0.654

0.720

1.000

1.104

1.839

1.870

1.972

2.032

2.070

2.600

3.458

3.775

3.852

3.914

H21

0.395

0.476

0.653

0.719

1.000

1.103

1.841

1.872

1.975

2.034

2.071

2.608

3.468

3.787

3.864

3.926

H22

0.388

0.473

0.651

0.717

1.000

1.103

1.834

1.864

1.968

2.027

2.064

2.597

3.456

3.775

3.851

3.914

H23

0.390

0.474

0.653

0.719

1.000

1.102

1.834

1.865

1.964

2.025

2.064

2.598

3.453

3.772

3.849

3.912

H24

0.391

0.474

0.652

0.718

1.000

1.103

1.832

1.864

1.967

2.025

2.062

2.596

3.452

3.770

3.846

3.909

H25

0.390

0.474

0.654

0.720

1.000

1.102

1.827

1.857

1.961

2.019

2.058

2.588

3.441

3.757

3.834

3.898

H26

0.390

0.474

0.654

0.721

1.000

1.103

1.832

1.863

1.962

2.023

2.060

2.594

3.452

3.769

3.846

3.908

H27

0.391

0.475

0.653

0.717

1.000

1.103

1.830

1.861

1.964

2.025

2.063

2.600

3.463

3.791

3.867

3.927

H28

0.390

0.475

0.653

0.716

1.000

1.103

1.833

1.864

1.968

2.029

2.067

2.604

3.469

3.798

3.874

3.936

H29

0.389

0.474

0.654

0.718

1.000

1.101

1.832

1.863

1.969

2.029

2.067

2.607

3.471

3.802

3.879

3.942

H30

0.390

0.474

0.654

0.718

1.000

1.101

1.834

1.865

1.970

2.031

2.069

2.607

3.472

3.803

3.880

3.943

H31

0.389

0.474

0.652

0.717

1.000

1.101

1.831

1.862

1.965

2.026

2.064

2.599

3.459

3.788

3.863

3.923

H32

0.389

0.473

0.650

0.716

1.000

1.101

1.831

1.862

1.965

2.026

2.064

2.599

3.461

3.790

3.867

3.930

H33

0.389

0.474

0.653

0.719

1.000

1.101

1.829

1.860

1.962

2.023

2.061

2.593

3.451

3.778

3.853

3.915

H34

0.389

0.474

0.652

0.713

1.000

1.103

1.835

1.866

1.969

2.031

2.068

2.603

3.464

3.794

3.870

3.932

H35

0.385

0.470

0.648

0.712

1.000

1.097

1.826

1.859

1.966

2.025

2.063

2.603

3.471

3.802

3.877

3.937

H36

0.388

0.471

0.652

0.716

1.000

1.103

1.830

1.862

1.966

2.027

2.065

2.604

3.470

3.801

3.876

3.938

H37

0.384

0.469

0.651

0.714

1.000

1.103

1.834

1.866

1.971

2.032

2.070

2.607

3.474

3.804

3.879

3.942

H38

0.392

0.475

0.655

0.718

1.000

1.104

1.830

1.861

1.964

2.025

2.063

2.597

3.456

3.785

3.860

3.921

H39

0.389

0.475

0.655

0.720

1.000

1.104

1.830

1.861

1.966

2.025

2.063

2.596

3.456

3.784

3.858

3.919

H40

0.391

0.475

0.656

0.719

1.000

1.103

1.828

1.859

1.962

2.023

2.060

2.593

3.451

3.776

3.852

3.914

H41

0.389

0.474

0.655

0.718

1.000

1.105

1.831

1.863

1.947

2.028

2.066

2.601

3.460

3.788

3.862

3.925

H42

0.390

0.474

0.654

0.719

1.000

1.103

1.828

1.860

1.963

2.023

2.060

2.593

3.449

3.776

3.852

3.911

H43

0.385

0.473

0.661

0.717

1.000

1.104

1.834

1.866

1.972

2.029

2.069

2.605

3.469

3.799

3.875

3.936

H44

0.388

0.474

0.661

0.718

1.000

1.104

1.831

1.862

1.973

2.028

2.066

2.602

3.464

3.792

3.870

3.930

H45

0.386

0.473

0.653

0.718

1.000

1.102

1.831

1.863

1.971

2.027

2.066

2.605

3.467

3.798

3.873

3.938

H46

0.385

0.472

0.652

0.715

1.000

1.102

1.835

1.867

1.971

2.030

2.069

2.604

3.463

3.795

3.870

3.934

H47

0.386

0.472

0.652

0.714

1.000

1.102

1.833

1.864

1.970

2.027

2.066

2.599

3.462

3.791

3.866

3.931

H48

0.385

0.472

0.652

0.717

1.000

1.102

1.835

1.866

1.973

2.028

2.068

2.603

3.464

3.792

3.867

3.933

H49

0.383

0.472

0.652

0.716

1.000

1.103

1.830

1.863

1.970

2.026

2.066

2.602

3.463

3.793

3.867

3.933

H50

0.385

0.472

0.651

0.716

1.000

1.101

1.831

1.863

1.966

2.024

2.064

2.599

3.461

3.790

3.865

3.930

H51

0.383

0.471

0.651

0.717

1.000

1.102

1.826

1.858

1.961

2.020

2.061

2.596

3.455

3.784

3.859

3.923

RSD/%

0.831

0.581

0.548

0.436

0.000

0.284

0.342

0.336

0.375

0.328

0.331

0.354

0.370

0.438

0.434

0.430

Component	Initial eigenvalue	Extract the sum of squares of the load
1	5.716	35.725	35.725	5.716	35.725	35.725
2	3.417	21.353	57.078	3.417	21.353	57.078
3	1.519	9.493	66.572	1.519	9.493	66.572
4	1.462	9.137	75.709	1.462	9.137	75.709

Component

Initial eigenvalue

Extract the sum of squares of the load

Total

Variance percentage

Cumulative variance contribution rate%

Total

Variance percentage

Cumulative variance contribution rate%

5.716

35.725

5.716

35.725

3.417

21.353

57.078

3.417

21.353

57.078

1.519

9.493

66.572

1.519

9.493

66.572

1.462

9.137

75.709

1.462

9.137

75.709