中国药学杂志

Batch No.	Harvest time
S1	-S6	2023-04-10
S7	-S12	2023-05-08
S13	-S18	2023-06-15
S19	-S24	2023-07-10
S25	-S30	2023-08-11
S31	-S36	2023-09-10
S37	-S42	2023-10-9
S43	-S48	2023-11-14
S49	-S54	2023-12-10

Batch No.	Harvest time
S1	-S6	2023-04-10
S7	-S12	2023-05-08
S13	-S18	2023-06-15
S19	-S24	2023-07-10
S25	-S30	2023-08-11
S31	-S36	2023-09-10
S37	-S42	2023-10-9
S43	-S48	2023-11-14
S49	-S54	2023-12-10

Index component	Linear range/μg·mL^-1	Regression equation	r
Echinacoside	0.126 1-2.018 5	Y=519 534X-578 699	0.999 5
Acteoside	0.129 8-2.077 3	Y=653 254X-56 740	0.999 4
Tubuloside A	0.015 5-0.248 2	Y=495 439X-43 588	0.999 4
Isoacteoside	0.025 3-0.405 9	Y=183 284X-26 016	0.999 2
Poliumoside	0.122 3-1.957 9	Y=112 458X-99 401	0.999 6
Geniposide	0.020 4-0.325 9	Y=325 746X-34 439	0.999 4

Index component	Linear range/μg·mL^-1	Regression equation	r
Echinacoside	0.126 1-2.018 5	Y=519 534X-578 699	0.999 5
Acteoside	0.129 8-2.077 3	Y=653 254X-56 740	0.999 4
Tubuloside A	0.015 5-0.248 2	Y=495 439X-43 588	0.999 4
Isoacteoside	0.025 3-0.405 9	Y=183 284X-26 016	0.999 2
Poliumoside	0.122 3-1.957 9	Y=112 458X-99 401	0.999 6
Geniposide	0.020 4-0.325 9	Y=325 746X-34 439	0.999 4

Indicator components	m(Sample)/g	m(Original)/mg	m(Added)/mg	m(Measured) /mg	Recovery rate/%	Average value/%	RSD/%
Echinacoside	0.250 1	0.574 4	0.584 5	1.172 5	102.33	101.31	1.78
	0.250 7	0.567 4	0.584 5	1.177 5	104.38
	0.251 4	0.588 4	0.584 5	1.174 5	100.27
	0.256 7	0.587 5	0.584 5	1.169 5	99.57
	0.264 1	0.588 0	0.584 5	1.172 5	100.00
	0.249 5	0.583 5	0.584 5	1.175 5	101.28
Acteoside	0.250 1	1.125 6	1.130 5	2.263 0	100.61	99.37	1.09
	0.250 7	1.147 4	1.130 5	2.265 5	98.90
	0.251 4	1.133 2	1.130 5	2.258 0	99.50
	0.256 7	1.134 5	1.130 5	2.256 0	99.20
	0.264 1	1.157 8	1.130 5	2.261 5	97.63
	0.249 5	1.132 2	1.130 5	2.267 0	100.38
Tubuloside A	0.250 1	0.585 5	0.589 7	1.182 0	101.15	101.54	1.43
	0.250 7	0.577 6	0.589 7	1.177 5	101.73
	0.251 4	0.584 3	0.589 7	1.185 0	101.87
	0.256 7	0.587 4	0.589 7	1.183 0	101.00
	0.264 1	0.577 4	0.589 7	1.190 5	103.97
	0.249 5	0.579 5	0.589 7	1.166 5	99.54
Isoacteoside	0.250 1	0.327 5	0.337 4	0.663 5	99.59	98.20	1.96
	0.250 7	0.345 6	0.337 4	0.667 0	95.26
	0.251 4	0.328 5	0.337 4	0.656 0	97.07
	0.256 7	0.332 5	0.337 4	0.672 5	100.77
	0.264 1	0.335 5	0.337 4	0.667 5	98.40
	0.249 5	0.332 5	0.337 4	0.663 5	98.10
Poliumoside	0.250 1	0.120 5	0.124 7	0.250 5	104.25	100.59	4.60
	0.250 7	0.129 1	0.124 7	0.256 0	101.76
	0.251 4	0.127 1	0.124 7	0.242 5	92.54
	0.256 7	0.122 5	0.124 7	0.244 5	97.83
	0.264 1	0.119 7	0.124 7	0.247 5	102.49
	0.249 5	0.120 5	0.124 7	0.251 0	104.65
Geniposide	0.250 1	1.957 5	1.966 7	3.952 5	101.44	99.81	1.05
	0.250 7	1.952 9	1.966 7	3.923 5	100.20
	0.251 4	1.944 5	1.966 7	3.918 0	100.35
	0.256 7	1.972 5	1.966 7	3.911 0	98.57
	0.264 1	1.952 5	1.966 7	3.899 5	99.00
	0.249 5	1.968 9	1.966 7	3.922 5	99.33

Indicator components	m(Sample)/g	m(Original)/mg	m(Added)/mg	m(Measured) /mg	Recovery rate/%	Average value/%	RSD/%
Echinacoside	0.250 1	0.574 4	0.584 5	1.172 5	102.33	101.31	1.78
	0.250 7	0.567 4	0.584 5	1.177 5	104.38
	0.251 4	0.588 4	0.584 5	1.174 5	100.27
	0.256 7	0.587 5	0.584 5	1.169 5	99.57
	0.264 1	0.588 0	0.584 5	1.172 5	100.00
	0.249 5	0.583 5	0.584 5	1.175 5	101.28
Acteoside	0.250 1	1.125 6	1.130 5	2.263 0	100.61	99.37	1.09
	0.250 7	1.147 4	1.130 5	2.265 5	98.90
	0.251 4	1.133 2	1.130 5	2.258 0	99.50
	0.256 7	1.134 5	1.130 5	2.256 0	99.20
	0.264 1	1.157 8	1.130 5	2.261 5	97.63
	0.249 5	1.132 2	1.130 5	2.267 0	100.38
Tubuloside A	0.250 1	0.585 5	0.589 7	1.182 0	101.15	101.54	1.43
	0.250 7	0.577 6	0.589 7	1.177 5	101.73
	0.251 4	0.584 3	0.589 7	1.185 0	101.87
	0.256 7	0.587 4	0.589 7	1.183 0	101.00
	0.264 1	0.577 4	0.589 7	1.190 5	103.97
	0.249 5	0.579 5	0.589 7	1.166 5	99.54
Isoacteoside	0.250 1	0.327 5	0.337 4	0.663 5	99.59	98.20	1.96
	0.250 7	0.345 6	0.337 4	0.667 0	95.26
	0.251 4	0.328 5	0.337 4	0.656 0	97.07
	0.256 7	0.332 5	0.337 4	0.672 5	100.77
	0.264 1	0.335 5	0.337 4	0.667 5	98.40
	0.249 5	0.332 5	0.337 4	0.663 5	98.10
Poliumoside	0.250 1	0.120 5	0.124 7	0.250 5	104.25	100.59	4.60
	0.250 7	0.129 1	0.124 7	0.256 0	101.76
	0.251 4	0.127 1	0.124 7	0.242 5	92.54
	0.256 7	0.122 5	0.124 7	0.244 5	97.83
	0.264 1	0.119 7	0.124 7	0.247 5	102.49
	0.249 5	0.120 5	0.124 7	0.251 0	104.65
Geniposide	0.250 1	1.957 5	1.966 7	3.952 5	101.44	99.81	1.05
	0.250 7	1.952 9	1.966 7	3.923 5	100.20
	0.251 4	1.944 5	1.966 7	3.918 0	100.35
	0.256 7	1.972 5	1.966 7	3.911 0	98.57
	0.264 1	1.952 5	1.966 7	3.899 5	99.00
	0.249 5	1.968 9	1.966 7	3.922 5	99.33

Batch No.	Echinacoside	Acteoside	Tubuloside A	Isoacteoside	Poliumoside	Geniposide
S1	0.548±0.006	0.637±0.012	0.232±0.017	0.637±0.015	0.045±0.002	0.095±0.002
S2	1.132±0.031	0.964±0.023	0.222±0.012	0.542±0.006	0.045±0.003	0.091±0.006
S3	0.858±0.014	0.841±0.027	0.237±0.051	0.643±0.011	0.048±0.001	0.056±0.003
S4	0.749±0.006	0.682±0.006	0.196±0.002	0.538±0.013	0.054±0.003	0.075±0.001
S5	0.972±0.024	0.766±0.022	0.283±0.016	0.479±0.024	0.038±0.001	0.065±0.003
S6	1.259±0.017	0.696±0.174	0.312±0.007	0.541±0.023	0.047±0.003	0.074±0.004
S7	1.128±0.007	0.895±0.003	0.383±0.016	0.755±0.010	0.043±0.001	0.064±0.004
S8	2.027±0.018	1.118±0.110	0.219±0.016	0.637±0.016	0.055±0.004	0.065±0.003
S9	1.358±0.006	1.150±0.017	0.337±0.053	0.535±0.005	0.044±0.002	0.094±0.003
S10	0.875±0.018	1.240±0.006	0.236±0.025	0.456±0.002	0.048±0.001	0.043±0.001
S11	1.247±0.008	0.958±0.024	0.232±0.008	0.419±0.006	0.051±0.001	0.043±0.003
S12	1.959±0.017	1.145±0.008	0.309±0.005	0.539±0.026	0.043±0.003	0.047±0.002
S13	0.758±0.023	0.669±0.022	0.189±0.011	0.442±0.033	0.053±0.001	0.088±0.001
S14	0.824±0.019	0.722±0.016	0.153±0.005	0.338±0.023	0.097±0.001	0.101±0.004
S15	0.644±0.018	0.536±0.026	0.205±0.003	0.314±0.002	0.063±0.005	0.116±0.008
S16	0.330±0.013	0.478±0.010	0.134±0.010	0.334±0.011	0.067±0.003	0.153±0.053
S17	0.764±0.010	0.548±0.012	0.246±0.035	0.353±0.034	0.058±0.001	0.096±0.001
S18	0.854±0.017	0.628±0.006	0.236±0.001	0.326±0.017	0.078±0.001	0.136±0.002
S19	0.530±0.006	0.561±0.014	0.182±0.014	0.331±0.016	0.063±0.001	0.145±0.003
S20	0.640±0.016	0.633±0.013	0.169±0.005	0.405±0.006	0.076±0.003	0.158±0.001
S21	0.543±0.020	0.455±0.023	0.143±0.036	0.295±0.004	0.086±0.001	0.134±0.002
S22	0.641±0.017	0.535±0.026	0.168±0.011	0.352±0.012	0.063±0.001	0.190±0.007
S23	0.936±0.012	0.413±0.002	0.219±0.024	0.330±0.030	0.054±0.003	0.154±0.002
S24	0.543±0.002	0.333±0.028	0.178±0.018	0.296±0.002	0.066±0.003	0.175±0.001
S25	0.537±0.012	0.552±0.034	0.151±0.024	0.362±0.004	0.046±0.003	0.155±0.003
S26	0.726±0.005	0.427±0.025	0.160±0.026	0.408±0.004	0.042±0.001	0.145±0.002
S27	0.425±0.011	0.573±0.005	0.148±0.005	0.342±0.008	0.036±0.004	0.137±0.002
S28	0.519±0.012	0.326±0.018	0.129±0.003	0.354±0.011	0.035±0.004	0.125±0.002
S29	0.337±0.023	0.420±0.013	0.151±0.008	0.322±0.007	0.046±0.001	0.157±0.001
S30	0.475±0.012	0.338±0.023	0.149±0.006	0.329±0.014	0.045±0.003	0.109±0.005
S31	0.166±0.012	0.263±0.043	0.094±0.003	0.306±0.003	0.033±0.002	0.196±0.001
S32	0.353±0.037	0.135±0.017	0.121±0.027	0.224±0.021	0.026±0.003	0.205±0.002
S33	0.531±0.010	0.257±0.021	0.133±0.027	0.275±0.012	0.035±0.003	0.195±0.003
S34	0.278±0.011	0.341±0.018	0.045±0.001	0.308±0.001	0.025±0.004	0.181±0.006
S35	0.359±0.024	0.349±0.006	0.112±0.011	0.260±0.017	0.024±0.003	0.174±0.003
S36	0.173±0.018	0.222±0.012	0.096±0.002	0.289±0.013	0.015±0.003	0.150±0.004
S37	0.236±0.036	0.369±0.027	0.013±0.001	0.250±0.016	0.025±0.002	0.182±0.006
S38	0.359±0.013	0.277±0.027	0.069±0.027	0.258±0.006	0.008±0.001	0.151±0.021
S39	0.129±0.006	0.156±0.021	0.068±0.022	0.308±0.001	0.016±0.001	0.167±0.001
S40	0.271±0.022	0.197±0.001	0.082±0.024	0.241±0.005	0.025±0.001	0.153±0.004
S41	0.241±0.006	0.226±0.018	0.052±0.005	0.205±0.001	0.024±0.004	0.165±0.004
S42	0.148±0.014	0.323±0.016	0.090±0.011	0.252±0.012	0.016±0.003	0.177±0.003
S43	0.467±0.019	0.364±0.017	0.122±0.002	0.314±0.016	0.025±0.002	0.235±0.037
S44	0.535±0.034	0.429±0.022	0.124±0.001	0.297±0.001	0.035±0.002	0.230±0.013
S45	0.252±0.033	0.480±0.021	0.124±0.001	0.315±0.001	0.035±0.004	0.308±0.005
S46	0.537±0.025	0.538±0.006	0.123±0.001	0.318±0.010	0.046±0.001	0.283±0.013
S47	0.635±0.006	0.332±0.032	0.152±0.005	0.296±0.007	0.052±0.001	0.308±0.001
S48	0.667±0.012	0.623±0.008	0.096±0.002	0.348±0.007	0.037±0.001	0.257±0.009
S49	0.813±0.001	0.731±0.028	0.103±0.001	0.322±0.003	0.046±0.004	0.292±0.005
S50	0.644±0.011	0.521±0.013	0.222±0.002	0.305±0.004	0.053±0.003	0.251±0.023
S51	0.548±0.023	0.464±0.034	0.130±0.006	0.366±0.003	0.061±0.003	0.312±0.002
S52	0.517±0.040	0.550±0.033	0.104±0.001	0.396±0.002	0.047±0.001	0.244±0.022
S53	0.633±0.012	0.630±0.017	0.087±0.003	0.354±0.010	0.053±0.004	0.220±0.010
S54	0.453±0.010	0.729±0.010	0.407±0.526	0.336±0.013	0.044±0.003	0.255±0.010

Batch No.	Echinacoside	Acteoside	Tubuloside A	Isoacteoside	Poliumoside	Geniposide
S1	0.548±0.006	0.637±0.012	0.232±0.017	0.637±0.015	0.045±0.002	0.095±0.002
S2	1.132±0.031	0.964±0.023	0.222±0.012	0.542±0.006	0.045±0.003	0.091±0.006
S3	0.858±0.014	0.841±0.027	0.237±0.051	0.643±0.011	0.048±0.001	0.056±0.003
S4	0.749±0.006	0.682±0.006	0.196±0.002	0.538±0.013	0.054±0.003	0.075±0.001
S5	0.972±0.024	0.766±0.022	0.283±0.016	0.479±0.024	0.038±0.001	0.065±0.003
S6	1.259±0.017	0.696±0.174	0.312±0.007	0.541±0.023	0.047±0.003	0.074±0.004
S7	1.128±0.007	0.895±0.003	0.383±0.016	0.755±0.010	0.043±0.001	0.064±0.004
S8	2.027±0.018	1.118±0.110	0.219±0.016	0.637±0.016	0.055±0.004	0.065±0.003
S9	1.358±0.006	1.150±0.017	0.337±0.053	0.535±0.005	0.044±0.002	0.094±0.003
S10	0.875±0.018	1.240±0.006	0.236±0.025	0.456±0.002	0.048±0.001	0.043±0.001
S11	1.247±0.008	0.958±0.024	0.232±0.008	0.419±0.006	0.051±0.001	0.043±0.003
S12	1.959±0.017	1.145±0.008	0.309±0.005	0.539±0.026	0.043±0.003	0.047±0.002
S13	0.758±0.023	0.669±0.022	0.189±0.011	0.442±0.033	0.053±0.001	0.088±0.001
S14	0.824±0.019	0.722±0.016	0.153±0.005	0.338±0.023	0.097±0.001	0.101±0.004
S15	0.644±0.018	0.536±0.026	0.205±0.003	0.314±0.002	0.063±0.005	0.116±0.008
S16	0.330±0.013	0.478±0.010	0.134±0.010	0.334±0.011	0.067±0.003	0.153±0.053
S17	0.764±0.010	0.548±0.012	0.246±0.035	0.353±0.034	0.058±0.001	0.096±0.001
S18	0.854±0.017	0.628±0.006	0.236±0.001	0.326±0.017	0.078±0.001	0.136±0.002
S19	0.530±0.006	0.561±0.014	0.182±0.014	0.331±0.016	0.063±0.001	0.145±0.003
S20	0.640±0.016	0.633±0.013	0.169±0.005	0.405±0.006	0.076±0.003	0.158±0.001
S21	0.543±0.020	0.455±0.023	0.143±0.036	0.295±0.004	0.086±0.001	0.134±0.002
S22	0.641±0.017	0.535±0.026	0.168±0.011	0.352±0.012	0.063±0.001	0.190±0.007
S23	0.936±0.012	0.413±0.002	0.219±0.024	0.330±0.030	0.054±0.003	0.154±0.002
S24	0.543±0.002	0.333±0.028	0.178±0.018	0.296±0.002	0.066±0.003	0.175±0.001
S25	0.537±0.012	0.552±0.034	0.151±0.024	0.362±0.004	0.046±0.003	0.155±0.003
S26	0.726±0.005	0.427±0.025	0.160±0.026	0.408±0.004	0.042±0.001	0.145±0.002
S27	0.425±0.011	0.573±0.005	0.148±0.005	0.342±0.008	0.036±0.004	0.137±0.002
S28	0.519±0.012	0.326±0.018	0.129±0.003	0.354±0.011	0.035±0.004	0.125±0.002
S29	0.337±0.023	0.420±0.013	0.151±0.008	0.322±0.007	0.046±0.001	0.157±0.001
S30	0.475±0.012	0.338±0.023	0.149±0.006	0.329±0.014	0.045±0.003	0.109±0.005
S31	0.166±0.012	0.263±0.043	0.094±0.003	0.306±0.003	0.033±0.002	0.196±0.001
S32	0.353±0.037	0.135±0.017	0.121±0.027	0.224±0.021	0.026±0.003	0.205±0.002
S33	0.531±0.010	0.257±0.021	0.133±0.027	0.275±0.012	0.035±0.003	0.195±0.003
S34	0.278±0.011	0.341±0.018	0.045±0.001	0.308±0.001	0.025±0.004	0.181±0.006
S35	0.359±0.024	0.349±0.006	0.112±0.011	0.260±0.017	0.024±0.003	0.174±0.003
S36	0.173±0.018	0.222±0.012	0.096±0.002	0.289±0.013	0.015±0.003	0.150±0.004
S37	0.236±0.036	0.369±0.027	0.013±0.001	0.250±0.016	0.025±0.002	0.182±0.006
S38	0.359±0.013	0.277±0.027	0.069±0.027	0.258±0.006	0.008±0.001	0.151±0.021
S39	0.129±0.006	0.156±0.021	0.068±0.022	0.308±0.001	0.016±0.001	0.167±0.001
S40	0.271±0.022	0.197±0.001	0.082±0.024	0.241±0.005	0.025±0.001	0.153±0.004
S41	0.241±0.006	0.226±0.018	0.052±0.005	0.205±0.001	0.024±0.004	0.165±0.004
S42	0.148±0.014	0.323±0.016	0.090±0.011	0.252±0.012	0.016±0.003	0.177±0.003
S43	0.467±0.019	0.364±0.017	0.122±0.002	0.314±0.016	0.025±0.002	0.235±0.037
S44	0.535±0.034	0.429±0.022	0.124±0.001	0.297±0.001	0.035±0.002	0.230±0.013
S45	0.252±0.033	0.480±0.021	0.124±0.001	0.315±0.001	0.035±0.004	0.308±0.005
S46	0.537±0.025	0.538±0.006	0.123±0.001	0.318±0.010	0.046±0.001	0.283±0.013
S47	0.635±0.006	0.332±0.032	0.152±0.005	0.296±0.007	0.052±0.001	0.308±0.001
S48	0.667±0.012	0.623±0.008	0.096±0.002	0.348±0.007	0.037±0.001	0.257±0.009
S49	0.813±0.001	0.731±0.028	0.103±0.001	0.322±0.003	0.046±0.004	0.292±0.005
S50	0.644±0.011	0.521±0.013	0.222±0.002	0.305±0.004	0.053±0.003	0.251±0.023
S51	0.548±0.023	0.464±0.034	0.130±0.006	0.366±0.003	0.061±0.003	0.312±0.002
S52	0.517±0.040	0.550±0.033	0.104±0.001	0.396±0.002	0.047±0.001	0.244±0.022
S53	0.633±0.012	0.630±0.017	0.087±0.003	0.354±0.010	0.053±0.004	0.220±0.010
S54	0.453±0.010	0.729±0.010	0.407±0.526	0.336±0.013	0.044±0.003	0.255±0.010

基于HPLC多成分含量测定结合化学计量学的荒漠肉苁蓉质量评价研究

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田利颖 ¹ , 李明杰 ² , 杨建华 ³ , 胡君萍 ¹^,⁴^,^*

中国药学杂志 | 论著 2025,60(9): 985-994

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中国药学杂志 |论著 2025 , 60 (9) : 985 -994

基于HPLC多成分含量测定结合化学计量学的荒漠肉苁蓉质量评价研究

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田利颖¹, 李明杰², 杨建华³, 胡君萍¹^,⁴^,^*

作者信息

¹ 新疆医科大学药学院, 乌鲁木齐 830017

² 沙雅县人民医院药剂科, 新疆沙雅 842200

³ 新疆医科大学第一附属医院, 乌鲁木齐 830011

⁴ 新疆生物药械重点实验室, 乌鲁木齐 830017

通讯作者:

^*胡君萍,女,博士,教授研究方向:天然产物的开发与应用 Tel:(0991)4363345

Quality Evaluation of Cistanche deserticola Based on HPLC Multi-Component Content Determination Combined with Chemometrics

Liying TIAN¹, Mingjie LI², Jianhua YANG³, Junping HU¹^,⁴^,^*

Affiliations

¹ School of Pharmacy, Xinjiang Medical University, Urumqi 830017, China

² Department of Pharmacy, Shaya County People's Hospital, Shaya 842200, China

³ The First Affiliated Hospital of Xinjiang Medical University, Urumqi 830011, China

⁴ Xinjiang Key Laboratory of Biopharmaceuticals and Medical Devices, Urumqi 830017, China

出版时间: 2025-05-01 doi: 10.11669/cpj.2025.09.011

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摘要

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目的研究荒漠肉苁蓉中有效成分在不同月份的积累规律,为荒漠肉苁蓉采收、产地加工和质量控制提供理论支持。方法采集2023年4~12月荒漠肉苁蓉样品54批,建立同时测定荒漠肉苁蓉中松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷和京尼平苷等6个成分含量的高效液相色谱(high performance liquid chromatography,HPLC)法,并对54批药材进行含量测定,分析其含量变化趋势。结合化学计量学分析,分别采用层次聚类分析(hierarchical cluster analysis,HCA)、主成分分析(principal component analysis,PCA)和正交偏最小二乘法-判别式分析(orthogonal partial least squares discriminant analysis,OPLS-DA)等对54批荒漠肉苁蓉药材进行鉴别和分类。结果所建立的HPLC方法能够使样品中的6个成分达到良好分离,苯乙醇苷类成分松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷含量随着药材开花在4~8月逐渐减少,在9~12月逐渐增高,而金石蚕苷含量在盛花期达到最高;环烯醚萜类成分京尼平苷在11~12月含量高于其他时期。从HCA和PCA分析中可发现54批荒漠肉苁蓉样品可明显区分为4类,其中春季采收期药材全部聚为一类,为伸长期(4~5月),主要特征为松果菊苷的含量较高;秋季采收期样品聚为一类,为裂果期(9~10月),主要特征为毛蕊花糖苷的含量较低;盛花期(6~8月)样品大部分聚为一类;所有休眠期(11~12月)样品聚为一类,主要特征是京尼平苷的含量较高,显示荒漠肉苁蓉药材在不同生长期成分含量有明显的差异。从OPLS-DA分析结果可以得出松果菊苷、毛蕊花糖苷是区分不同生长期贡献较大的两种成分,可作为评价荒漠肉苁蓉药材质量的指标性成分,从而进一步对不同生长期进行区分。结论本研究建立的HPLC方法准确度良好,结合化学计量分析,可用于区分不同月份荒漠肉苁蓉药材质量的差异性,为其采收及质量控制提供参考。

关键词

荒漠肉苁蓉 / 质量评价 / 化学计量学 / 松果菊苷 / 毛蕊花糖苷 / 管花苷A / 异毛蕊花糖苷

Abstract

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OBJECTIVE To study the accumulation pattern of effective components in Cistanche deserticola in different months, and to provide theoretical support for the harvesting, processing and quality control of Cistanche deserticola. METHODS Fifty-four batches of Cistanche deserticola samples were collected from April to December 2023, and a high performance liquid chromatography(HPLC) method was established for the simultaneous determination of six components in Cistanche deserticola, such as echinacoside, acteoside, tubuloside A, isoacteoside, poliumoside and geniposide, etc. The content of 54 batches of herbs were determined to analyze the trend of content changes. 54 batches of Cistanche deserticola herbs were identified and classified by chemometrics analysis, hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA). RESULTS The established HPLC method was able to achieve a good separation of six components in the samples. The contents of the echinacoside, acteoside, tubuloside A, and isoacteoside, decreased gradually with the blooming of the herbs in April-August and increased in September-December while the contents of poliumoside decreased in the blooming stage of Cistanche deserticola. The content of geniposide reached its highest in the full bloom period; the content of the cyclic enol ether terpene constituent geniposide was higher in November-December than in the other periods. From the HCA and PCA analyses, it was found that 54 batches of Cistanche deserticola samples could be clearly differentiated into four groups(elongation period, full bloom period, fruit splitting period, and dormant period), among which all of them were clustered together in one group during the spring harvesting period, and the main feature was that the content of echinacoside was the highest; the samples of Cistanche deserticola samples were clustered together in one group during the autumn harvesting period, and the main feature was the lowest content of acteoside; most of the Cistanche deserticola samples at the full bloom stage were clustered into one group; all the samples at the dormant stage were clustered into one group, and the main characteristic was the highest content of geniposide.The results showed that the contents of the constituents in different growth stages of the herbs of Cistanche deserticola were significantly different. From the results of OPLS-DA analysis, it can be concluded that echinacoside and acteoside are the two components that contribute more to the different growth periods, which are the key components to distinguish the different growth periods, and can be used as the index components for evaluating the quality of Cistanche deserticola herbs, so as to further differentiate the different growth periods. CONCLUSION The HPLC method established in this study has good accuracy, and combined with chemometric analysis, it can be used to distinguish the differences in the quality of the herbs of Cistanche deserticola in different months, and provide a reference for its harvesting and quality control.

Key words

Cistanche deserticola / quality assessment / chemometrics / echinacoside / acteoside / tubuloside A / isoacteoside

引用本文

田利颖, 李明杰, 杨建华, 胡君萍. 基于HPLC多成分含量测定结合化学计量学的荒漠肉苁蓉质量评价研究. 中国药学杂志, 2025 , 60 (9) : 985 -994 . DOI: 10.11669/cpj.2025.09.011

Liying TIAN, Mingjie LI, Jianhua YANG, Junping HU. Quality Evaluation of Cistanche deserticola Based on HPLC Multi-Component Content Determination Combined with Chemometrics[J]. Chinese Pharmaceutical Journal, 2025 , 60 (9) : 985 -994 . DOI: 10.11669/cpj.2025.09.011

正文

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肉苁蓉俗称大芸,为列当科多年生草本寄生植物荒漠肉苁蓉(Cistanche deserticola Y. C. Ma.)和管花肉苁蓉[Cistanche tubulosa(Schenk)Wight]干燥带鳞叶的肉质茎,最早记载于《神农本草经》,列为上品^[1]。荒漠肉苁蓉为我国干旱地区特有的沙生濒危药材,被历代医书古籍所收载,并具有药食两用历史^[2]。具有补肾阳、益精血、润肠通便的功效,可用于阳痿、遗精、早泄、腰膝冷痛等,素有“沙漠人参”之称^[3]。

荒漠肉苁蓉活性成分丰富,主要含有苯乙醇苷类^[4]、环烯醚萜类^[5]、挥发性成分^[6]、生物碱^[7]、多糖^[8]、黄酮^[9]及酚酸^[10]等成分。苯乙醇苷是荒漠肉苁蓉中的主要有效成分,也是研究荒漠肉苁蓉化学组分中报道最多的一类化合物,具有保护神经、护肝、抗疲劳、改善衰老等多种药理活性^[11]。目前在肉苁蓉中发现的苯乙醇苷有近50种,其中含量最多是松果菊苷和毛蕊花糖苷。此外,松果菊苷和毛蕊花糖苷也是《中国药典》2020年版规定的指标成分^[12],具有保护神经及改善记忆^[13]、调节细胞增殖^[14]等多种生理活性。事实上,除松果菊苷和毛蕊花糖苷外,荒漠肉苁蓉中还含有管花苷A、异毛蕊花糖苷、京尼平苷、金石蚕苷等有效成分,具有抗氧化^[15]、抗炎、抗肿瘤、神经保护^[16]及免疫调节^[17]等作用。这些成分都对荒漠肉苁蓉药效的发挥起到了重要作用。

肉苁蓉的品质与其化学成分的关联性是研究的焦点。研究表明,不同月份采收的肉苁蓉有效成分含量存在差异,有研究报道不同采收期肉苁蓉中松果菊苷、毛蕊花糖苷含量差异较大^[18]。这种差异可能与植物生长周期、气候条件等因素有关。目前荒漠肉苁蓉多在春季(4~5月)及秋季(9~10月)采收,针对荒漠肉苁蓉的大部分研究主要集中在采收期肉质茎中松果菊苷和毛蕊花糖苷含量变化上,对其生命周期其他化学成分的含量差异研究尚未见报道。通过对不同月份采收的肉苁蓉进行含量测定,可以揭示其化学成分的季节性变化规律,这对于优化采收时间和提高药材品质具有重要意义。

本研究选取松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷和京尼平苷等6种成分作为质量控制指标,通过对2023年4~12月采收的54批荒漠肉苁蓉药材进行含量测定及差异比较分析,跟踪荒漠肉苁蓉药材发育过程中各成分的动态变化,为新疆荒漠肉苁蓉质量整体评价提供参考,也为荒漠肉苁蓉农业生产、质量控制和资源合理利用等提供理论数据支持。

1 仪器与药材

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1.1 试剂

对照品松果菊苷(纯度≥98%,批号:PCL-#-A003)、毛蕊花糖苷(纯度≥98%,批号:PCL-#-M235)、管花苷A(纯度≥99%,批号:PCL-#-T003)、金石蚕苷(纯度≥99%,批号:PCL-#-D005)、异毛蕊花糖苷(纯度≥98%,批号:PCL-#-I236)(四川普西奥标物科技有限公司);对照品京尼平苷(纯度≥98%,批号:WP23120502);甲醇、乙腈为色谱纯。

1.2 仪器与设备

LC-20A型高效液相色谱仪(日本岛津公司);紫外可见分光光度计(上海佑科仪器仪表有限公司);DHG-9246A型电热恒温鼓风干燥箱(上海精宏实验设备有限公司);Plusel+Chorusl超纯水仪(法国威立雅公司)。

1.3 药材

新鲜的荒漠肉苁蓉样品于2023年4~12月采集于新疆阿克苏地区,样品经沙雅县人民医院李明杰主任药师鉴定为列当科肉苁蓉属植物荒漠肉苁蓉(Cistanche deserticola Y.C.Ma.)的干燥带鳞叶的肉质茎。各批次采用严格的前处理流程:去除表面杂质后,切片,于60 ℃电热恒温鼓风干燥箱中干燥至恒重,凭证标本保存于新疆医科大学生药学研究室。具体样品信息见表1。

2 方法与结果

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2.1 色谱条件

参考文献[19]方法并作优化。色谱柱:HypersilODS-2柱(4.6 mm×250 mm,5 μm);流动相:乙腈(A)-0.4%磷酸水溶液(B)梯度洗脱;流速:0.75 mL·min^-1;柱温:25 ℃;进样量:10 μL;洗脱梯度为:0~20 min,15%→20%A;20~30 min,20%→30%A;30~35 min,30%→15%A。检测波长:333 nm。

2.2 溶液的制备

2.2.1 对照品溶液的制备

精密称取松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷对照品适量,加体积分数50%甲醇制成混合对照品溶液,摇匀,即得。

2.2.2 供试品溶液的制备

取荒漠肉苁蓉粉末约1 g[粉碎,用65目四号药筛过筛,筛孔内径(250 ±9.9)μm],精密称定,置于100 mL棕色量瓶中,精密加入体积分数50%甲醇50 mL,密塞,摇匀,称定质量,浸泡30 min,超声处理40 min(功率250 W,频率35 kHz),放冷,再称定质量,加体积分数50%甲醇补足减失的质量,摇匀,静置,取上清液,经0.22 μm微孔滤膜滤过,取续滤液,即得。

2.3 方法学考察

2.3.1 空白试验

按照“2.1”项下色谱条件测定混合对照品溶液、荒漠肉苁蓉样品(S1)供试品溶液和空白溶剂,结果表明样品中各成分分离度与响应值均较好,且空白样品溶液无干扰(图1)。

2.3.2 线性关系考察

精密称取松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷对照品适量,制成每1 mL含松果菊苷25.232 μg、毛蕊花糖苷25.967 μg、管花苷A 3.102 μg、异毛蕊花糖苷5.074 μg、金石蚕苷24.474 μg和京尼平苷4.074 μg的混合对照品贮备溶液。分别精密移取上述对照品贮备溶液0.05、0.10、0.20、0.40、0.60、0.80 mL,分别置于10 mL量瓶中,加体积分数50%甲醇制成每1 mL含松果菊苷0.126、0.252、0.504、1.009、1.513、2.018 μg,毛蕊花糖苷0.129、0.259、0.519、1.038、1.558、2.077 μg,管花苷A0.015、0.031、0.062、0.124、0.186、0.248 μg,异毛蕊花糖苷0.025、0.050、0.101、0.202、0.304、0.405 μg,金石蚕苷0.122、0.244、0.489、0.978、1.468、1.957 μg,京尼平苷0.020、0.040、0.081、0.162、0.244、0.325 μg的混合对照品溶液,依次精密吸取上述混合对照品贮备液和应用液各10 μL,按“2.1”项下色谱条件进样测定,以峰面积(Y)为纵坐标,以对照品浓度(X)为横坐标,绘制标准曲线,结果见表2,相关系数r均大于0.999 0,表明各成分在规定的浓度范围内,峰面积与对照品浓度线性关系良好。

2.3.3 精密度试验

取混合标准品连续进样6次,测定峰面积,松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷峰面积相对标准偏差(RSD)值分别为1.81%、1.22%、1.67%、1.76%、1.62%、1.45%,表明该仪器精密度良好。

2.3.4 稳定性试验

取同一份荒漠肉苁蓉样品(S1),分别于样品制备后的0、2、4、8、12、18、24 h进样,按“2.1”项下色谱条件测定。结果发现,荒漠肉苁蓉样品溶液中松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷峰面积RSD值分别为1.92%、2.71%、0.38%、2.02%、1.44%、0.46%,表明供试品溶液在24 h内稳定性良好。

2.3.5 重复性试验

取同一份荒漠肉苁蓉样品(S1)约0.5 g,精密称定,按“2.2.2”项下方法平行制备供试品溶液6份,按“2.1”项下色谱条件测定。结果显示,荒漠肉苁蓉样品溶液中松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷峰面积RSD值分别为0.24%、0.55%、0.26%、2.84%、0.76%、2.55%,表明重复性良好。

2.3.6 加样回收率试验

分别称取6份已知含量的荒漠肉苁蓉样品(S1)约0.25 g,精密称定,置于具塞锥形瓶中,分别加入一定量的松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷对照品溶液,按“2.2.2”项下方法制备供试品溶液,测定溶液中的松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷含量并计算加样回收率,结果见表3,回收率RSD均小于5%,符合规定,表明该分析方法准确度良好。

2.4 样品测定

取54批各个月份的荒漠肉苁蓉药材粉末,按“2.2.2”项下方法制备供试品溶液,按“2.1”项下色谱条件测定,采用外标法进行计算,54批荒漠肉苁蓉药材中6个成分含量测定数据结果见表4。结果显示54批荒漠肉苁蓉药材中松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷、京尼平苷含量范围分别为0.129%~2.027%、0.135%~1.240%、0.013%~0.407%、0.205%~0.755%、0.008%~0.097%、0.043%~0.312%。不同月份6个指标成分含量变化趋势见图2,结果显示,在春季采收期(4~5月)松果菊苷、毛蕊花糖苷、管花苷、异毛蕊花糖苷含量呈现上升趋势,随着月份变化,气温逐渐变暖,植株开花,其含量逐渐降低,到秋季采收期(9~10月)达到最低点,然后气温逐渐降低,植株进入半休眠状态,含量积累呈现整体上升趋势;而金石蚕苷含量在春季采收期及盛花期含量逐渐增高达到峰值,后逐渐降低;京尼平苷含量则随着季节的变化含量逐渐增高,在休眠期达到最高点。

2.5 化学模式识别分析

2.5.1 聚类分析(HCA)

以54批不同生长期荒漠肉苁蓉样品中6个成分的含量为数据源,利用IBM SPSS Statistics 26.0软件进行min~max标准化处理,再应用origin 2021软件以平方欧式距离进行层次聚类^[20],见图3。结果显示,所有54批样品被聚为4类,其中12批春季采收期样品(S1~S12)聚为一类,主要特征为松果菊苷的含量最高(范围为0.548%~2.027%);12批秋季采收期样品(S31~S42)聚为一类,主要特征为毛蕊花糖苷的含量最低(范围为0.135%~0.369%);12批休眠期样品(S43~S54)大致聚为一类,主要特征是京尼平苷的含量最高(0.220%~0.320%);18批盛花期样品(S13~S30)聚为一类。说明通过HCA可大致区分荒漠肉苁蓉不同生长期的样品。

2.5.2 主成分分析(PCA)

为更好地将不同生长期荒漠肉苁蓉进行区分,另采用PCA进行分析,PCA可实现高维数据的降维处理,少数几个主成分(综合变量)即可代原始数据的大部分信息^[21-22]。同样以54批不同生长期荒漠肉苁蓉药材6个成分含量为原始数据,导入SIMCA 14.1软件绘制54批不同生长期荒漠肉苁蓉样品的主成分得分图,生成3个主成分,累积贡献率为0.963,Q²为0.941,Q²大于0.5证明模型有效,以前两个主成分的得分值为X、Y值,生成PCA得分图(图4)。结果显示,PCA按生长期的不同,将54批荒漠肉苁蓉大致分为4类,其中12批春季采收期荒漠肉苁蓉(S1~S12)为A类,主要特征为松果菊苷及毛蕊花糖苷含量较高(总含量为1.181%~3.267%);18批盛花期(S13~S30)为B类,主要特征为金石蚕苷含量最高(0.035%~0.097%);12批秋季采收期荒漠肉苁蓉(S31~S42)为C类,主要特征为松果菊苷及毛蕊花糖苷含量较低(0.27%~0.91%);12批休眠期荒漠肉苁蓉(S43~S54)为D类,主要特征是京尼平苷的含量最高(0.220%~0.320%)。盛花期和生长期荒漠肉苁蓉在PCA得分图上分布较为接近,而春季采收期及秋季采收期荒漠肉苁蓉,在主成分得分上与盛花期和生长期荒漠肉苁蓉的差异较大,说明荒漠肉苁蓉在采收期前后化学成分的含量存在较大变化,该结果与HCA基本一致。

2.5.3 正交偏最小二乘法判别式分析(OPLS-DA)

为更好地观察不同生长期荒漠肉苁蓉样品之间的组内差异^[23],进一步采用有监督的OPLS-DA模型进行分析。以样品S1~S54为Y变量,6种成分的含量为X变量,利用SIMCA 14.1软件进行OPLS-DA处理。结果在建立的偏最小二乘判别分析模型中R²X(cum)=0.961,R²Y(cum)=0.976,Q²(cum)=0.865,均大于0.5,说明建立的OPLS-DA模型解释率和预测力可靠、良好,见图5。结果显示,54批样品分为4类,4个生长期各聚为一类,表明这6个成分在评价样品不同生长期之间的质量差异具有重要参考价值。同时,结合变量重要性投影值(variable importance in projection,VIP)值越大,表明对样品分类贡献较大^[24]。图6中VIP>1的有两种成分,为松果菊苷和毛蕊花糖苷,说明这两种成分是影响不同生长期样品之间质量差异贡献较大的成分,可见《中国药典》2020年版将松果菊苷和毛蕊花糖苷作为指导荒漠肉苁蓉药材质量控制的关键成分是科学的。

2.5.4 不同生长期6个指标成分平均含量分布图

不同生长期6个指标成分含量的均值对比见图7,结果显示苯乙醇苷类成分松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷均在春季采收期含量占比最高,秋季采收期含量占比最低;金石蚕苷则在盛花期含量较高,而环烯醚萜苷类成分京尼平苷在秋季采收期占比最高,春季采收期占比最低。

3 讨论

收起

由于中药材含有多种复杂成分,其质量控制不易。目前主要通过检测某些特定成分来评估中药材质量,但这种方法不够全面。中药材的有效成分是其生长时产生的次生代谢产物,这些成分的积累决定了药材的质量。中药材生产既要追求产量,也要保证质量,但产量和有效成分含量的变化往往不一致,这让确定最佳采收时间变得困难。研究荒漠肉苁蓉整个生长过程中有效成分的变化,可以帮助我们更准确地评估其质量,并为生产和质量控制提供科学依据^[25]。

本研究含量测定结果显示,不同采收期荒漠肉苁蓉药材中松果菊苷、毛蕊花糖苷等主要苯乙醇苷类成分的含量在春季采收期(4~5月)最高,在盛花期(6~8月)逐渐降低,在秋季采收期(9~10月)含量达到最低,随后含量在生长期(11~12月)逐渐增长;金石蚕苷在盛花期含量最高,而环烯醚萜类成分京尼平苷则在生长期最高。其中苯乙醇苷类成分的含量变化与文献报道的趋势一致,即春季采收期苯乙醇苷含量明显高于秋季采收期^[26]。含量变化可能是开花导致肉苁蓉根茎中空而降低其质量,在地下生长的时期为肉苁蓉成分累积阶段,活性成分丰富;而开花后肉苁蓉表面呈浅灰色或黄棕色、鳞片稀疏、干瘪,活性成分逐渐降低^[27]。据报道,荒漠肉苁蓉秋季采收期也被称为油苁蓉,多糖含量较高,秋季样品量显著高于春季样品,多糖是本药材具有较强的润肠通便作用的物质基础^[28]。由此可见可对不同采收期的荒漠肉苁蓉进行不同的产地加工,春季采收期药材可作为天然的抗氧化物资源进行研究,秋季采收期药材可偏向于润肠通便药物进行开发。

近年利用中药多成分测定结合化学模式识别分析中药样品的差异,在中药质量评价研究应用中较为广泛^[29]。本研究通过同时测定54批荒漠肉苁蓉中6个成分含量,并结合化学模式进行分析,探索了鉴别不同生长期荒漠肉苁蓉药材的方法。在HCA分析结果中,4个生长期的荒漠肉苁蓉样品分别聚为4类,其中春季采收期荒漠肉苁蓉全部聚为一类,主要特征为松果菊苷的含量最高;秋季采收期荒漠肉苁蓉样品聚为一类,主要特征为毛蕊花糖苷的含量最低;盛花期荒漠肉苁蓉样品大部分聚为一类;所有休眠期样品聚为一类,主要特征是京尼平苷的含量最高,结果表明荒漠肉苁蓉药材的不同生长期成分含量有明显的差异。结合PCA和OPLS-DA进一步分析了不同生长期荒漠肉苁蓉的质量差异标志物,结果显示,4个不同生长期的荒漠肉苁蓉样品均明显位于空间的不同位置,反映了荒漠肉苁蓉样品不同生长期间的差异。同时发现松果菊苷、毛蕊花糖苷两种苯乙醇苷类成分是区分不同生长期样品贡献较大的差异性成分,这与上述荒漠肉苁蓉不同生长期主要苯乙醇苷类成分含量有所差异的结论相符。

根据文献[19],苯乙醇苷类物质的最大吸收波长为333 nm。本实验测得333 nm可使松果菊苷、毛蕊花糖苷、管花苷A、异毛蕊花糖苷、金石蚕苷和京尼平苷等6个指标成分同时存在较强的吸收峰,而其他成分的吸收较弱或无吸收,能够有效区分这些物质及其他杂质。然而,样品中还出现了未测得的吸收度较大的未知峰。这些未知峰可能是由样品不纯、色谱柱污染、流动相问题或仪器参数设置不当引起的。在未明确鉴定这些未知峰成分之前,暂时忽略它们来评价样品的质量。后续实验会进一步鉴定这些成分,以确保分析结果的全面性和准确性。

综上,本研究建立了荒漠肉苁蓉药材多个成分的含量测定方法,为荒漠肉苁蓉药材的质量标准提升提供了重要参考。通过对不同生长期荒漠肉苁蓉中6种成分的含量比较,跟踪荒漠肉苁蓉药材中化学组分的积累规律,为荒漠肉苁蓉药材质量的客观评价和控制提供数据支撑。同时结合化学计量学的分析,揭示了苯乙醇苷类成分在荒漠肉苁蓉不同生长期的差异,对其进行质量控制,进而为新疆荒漠肉苁蓉质量整体评价提供参考,也为荒漠肉苁蓉农业生产、质量控制和资源合理利用等提供理论数据支持。

基金

收起

新疆维吾尔自治区自然科学基金重点项目资助(2021D01D11)
新疆维吾尔自治区自然科学基金重点项目资助(2022D01D14)
新疆维吾尔自治区自然科学基金地州科学基金项目资助(2022D01F92)
新疆天然药物有效成分与药物释放技术重点实验室项目资助(XJDX1713)

参考文献

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文献

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2025年第60卷第9期

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文章信息

doi: 10.11669/cpj.2025.09.011

接收时间：2025-01-17
首发时间：2025-11-11
出版时间：2025-05-01

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收稿日期：2025-01-17

基金

新疆维吾尔自治区自然科学基金重点项目资助(2021D01D11)

新疆维吾尔自治区自然科学基金重点项目资助(2022D01D14)

新疆维吾尔自治区自然科学基金地州科学基金项目资助(2022D01F92)

新疆天然药物有效成分与药物释放技术重点实验室项目资助(XJDX1713)

作者信息

¹ 新疆医科大学药学院, 乌鲁木齐 830017

² 沙雅县人民医院药剂科, 新疆沙雅 842200

³ 新疆医科大学第一附属医院, 乌鲁木齐 830011

⁴ 新疆生物药械重点实验室, 乌鲁木齐 830017

通讯作者:

^*胡君萍,女,博士,教授研究方向:天然产物的开发与应用 Tel:(0991)4363345

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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

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Batch No.	Harvest time
S1	-S6	2023-04-10
S7	-S12	2023-05-08
S13	-S18	2023-06-15
S19	-S24	2023-07-10
S25	-S30	2023-08-11
S31	-S36	2023-09-10
S37	-S42	2023-10-9
S43	-S48	2023-11-14
S49	-S54	2023-12-10

Batch No.

Harvest time

-S6

2023-04-10

-S12

2023-05-08

S13

-S18

2023-06-15

S19

-S24

2023-07-10

S25

-S30

2023-08-11

S31

-S36

2023-09-10

S37

-S42

2023-10-9

S43

-S48

2023-11-14

S49

-S54

2023-12-10

Index component	Linear range/μg·mL^-1	Regression equation	r
Echinacoside	0.126 1-2.018 5	Y=519 534X-578 699	0.999 5
Acteoside	0.129 8-2.077 3	Y=653 254X-56 740	0.999 4
Tubuloside A	0.015 5-0.248 2	Y=495 439X-43 588	0.999 4
Isoacteoside	0.025 3-0.405 9	Y=183 284X-26 016	0.999 2
Poliumoside	0.122 3-1.957 9	Y=112 458X-99 401	0.999 6
Geniposide	0.020 4-0.325 9	Y=325 746X-34 439	0.999 4

Index component

Linear range/μg·mL^-1

Regression equation

Echinacoside

0.126 1-2.018 5

Y=519 534X-578 699

0.999 5

Acteoside

0.129 8-2.077 3

Y=653 254X-56 740

0.999 4

Tubuloside A

0.015 5-0.248 2

Y=495 439X-43 588

0.999 4

Isoacteoside

0.025 3-0.405 9

Y=183 284X-26 016

0.999 2

Poliumoside

0.122 3-1.957 9

Y=112 458X-99 401

0.999 6

Geniposide

0.020 4-0.325 9

Y=325 746X-34 439

0.999 4

Indicator components	m(Sample)/g	m(Original)/mg	m(Added)/mg	m(Measured) /mg	Recovery rate/%	Average value/%	RSD/%
Echinacoside	0.250 1	0.574 4	0.584 5	1.172 5	102.33	101.31	1.78
	0.250 7	0.567 4	0.584 5	1.177 5	104.38
	0.251 4	0.588 4	0.584 5	1.174 5	100.27
	0.256 7	0.587 5	0.584 5	1.169 5	99.57
	0.264 1	0.588 0	0.584 5	1.172 5	100.00
	0.249 5	0.583 5	0.584 5	1.175 5	101.28
Acteoside	0.250 1	1.125 6	1.130 5	2.263 0	100.61	99.37	1.09
	0.250 7	1.147 4	1.130 5	2.265 5	98.90
	0.251 4	1.133 2	1.130 5	2.258 0	99.50
	0.256 7	1.134 5	1.130 5	2.256 0	99.20
	0.264 1	1.157 8	1.130 5	2.261 5	97.63
	0.249 5	1.132 2	1.130 5	2.267 0	100.38
Tubuloside A	0.250 1	0.585 5	0.589 7	1.182 0	101.15	101.54	1.43
	0.250 7	0.577 6	0.589 7	1.177 5	101.73
	0.251 4	0.584 3	0.589 7	1.185 0	101.87
	0.256 7	0.587 4	0.589 7	1.183 0	101.00
	0.264 1	0.577 4	0.589 7	1.190 5	103.97
	0.249 5	0.579 5	0.589 7	1.166 5	99.54
Isoacteoside	0.250 1	0.327 5	0.337 4	0.663 5	99.59	98.20	1.96
	0.250 7	0.345 6	0.337 4	0.667 0	95.26
	0.251 4	0.328 5	0.337 4	0.656 0	97.07
	0.256 7	0.332 5	0.337 4	0.672 5	100.77
	0.264 1	0.335 5	0.337 4	0.667 5	98.40
	0.249 5	0.332 5	0.337 4	0.663 5	98.10
Poliumoside	0.250 1	0.120 5	0.124 7	0.250 5	104.25	100.59	4.60
	0.250 7	0.129 1	0.124 7	0.256 0	101.76
	0.251 4	0.127 1	0.124 7	0.242 5	92.54
	0.256 7	0.122 5	0.124 7	0.244 5	97.83
	0.264 1	0.119 7	0.124 7	0.247 5	102.49
	0.249 5	0.120 5	0.124 7	0.251 0	104.65
Geniposide	0.250 1	1.957 5	1.966 7	3.952 5	101.44	99.81	1.05
	0.250 7	1.952 9	1.966 7	3.923 5	100.20
	0.251 4	1.944 5	1.966 7	3.918 0	100.35
	0.256 7	1.972 5	1.966 7	3.911 0	98.57
	0.264 1	1.952 5	1.966 7	3.899 5	99.00
	0.249 5	1.968 9	1.966 7	3.922 5	99.33

Indicator components

m(Sample)/g

m(Original)/mg

m(Added)/mg

m(Measured) /mg

Recovery rate/%

Average value/%

RSD/%

Echinacoside

0.250 1

0.574 4

0.584 5

1.172 5

102.33

101.31

1.78

0.250 7

0.567 4

0.584 5

1.177 5

104.38

0.251 4

0.588 4

0.584 5

1.174 5

100.27

0.256 7

0.587 5

0.584 5

1.169 5

99.57

0.264 1

0.588 0

0.584 5

1.172 5

100.00

0.249 5

0.583 5

0.584 5

1.175 5

101.28

Acteoside

0.250 1

1.125 6

1.130 5

2.263 0

100.61

99.37

1.09

0.250 7

1.147 4

1.130 5

2.265 5

98.90

0.251 4

1.133 2

1.130 5

2.258 0

99.50

0.256 7

1.134 5

1.130 5

2.256 0

99.20

0.264 1

1.157 8

1.130 5

2.261 5

97.63

0.249 5

1.132 2

1.130 5

2.267 0

100.38

Tubuloside A

0.250 1

0.585 5

0.589 7

1.182 0

101.15

101.54

1.43

0.250 7

0.577 6

0.589 7

1.177 5

101.73

0.251 4

0.584 3

0.589 7

1.185 0

101.87

0.256 7

0.587 4

0.589 7

1.183 0

101.00

0.264 1

0.577 4

0.589 7

1.190 5

103.97

0.249 5

0.579 5

0.589 7

1.166 5

99.54

Isoacteoside

0.250 1

0.327 5

0.337 4

0.663 5

99.59

98.20

1.96

0.250 7

0.345 6

0.337 4

0.667 0

95.26

0.251 4

0.328 5

0.337 4

0.656 0

97.07

0.256 7

0.332 5

0.337 4

0.672 5

100.77

0.264 1

0.335 5

0.337 4

0.667 5

98.40

0.249 5

0.332 5

0.337 4

0.663 5

98.10

Poliumoside

0.250 1

0.120 5

0.124 7

0.250 5

104.25

100.59

4.60

0.250 7

0.129 1

0.124 7

0.256 0

101.76

0.251 4

0.127 1

0.124 7

0.242 5

92.54

0.256 7

0.122 5

0.124 7

0.244 5

97.83

0.264 1

0.119 7

0.124 7

0.247 5

102.49

0.249 5

0.120 5

0.124 7

0.251 0

104.65

Geniposide

0.250 1

1.957 5

1.966 7

3.952 5

101.44

99.81

1.05

0.250 7

1.952 9

1.966 7

3.923 5

100.20

0.251 4

1.944 5

1.966 7

3.918 0

100.35

0.256 7

1.972 5

1.966 7

3.911 0

98.57

0.264 1

1.952 5

1.966 7

3.899 5

99.00

0.249 5

1.968 9

1.966 7

3.922 5

99.33

Batch No.	Echinacoside	Acteoside	Tubuloside A	Isoacteoside	Poliumoside	Geniposide
S1	0.548±0.006	0.637±0.012	0.232±0.017	0.637±0.015	0.045±0.002	0.095±0.002
S2	1.132±0.031	0.964±0.023	0.222±0.012	0.542±0.006	0.045±0.003	0.091±0.006
S3	0.858±0.014	0.841±0.027	0.237±0.051	0.643±0.011	0.048±0.001	0.056±0.003
S4	0.749±0.006	0.682±0.006	0.196±0.002	0.538±0.013	0.054±0.003	0.075±0.001
S5	0.972±0.024	0.766±0.022	0.283±0.016	0.479±0.024	0.038±0.001	0.065±0.003
S6	1.259±0.017	0.696±0.174	0.312±0.007	0.541±0.023	0.047±0.003	0.074±0.004
S7	1.128±0.007	0.895±0.003	0.383±0.016	0.755±0.010	0.043±0.001	0.064±0.004
S8	2.027±0.018	1.118±0.110	0.219±0.016	0.637±0.016	0.055±0.004	0.065±0.003
S9	1.358±0.006	1.150±0.017	0.337±0.053	0.535±0.005	0.044±0.002	0.094±0.003
S10	0.875±0.018	1.240±0.006	0.236±0.025	0.456±0.002	0.048±0.001	0.043±0.001
S11	1.247±0.008	0.958±0.024	0.232±0.008	0.419±0.006	0.051±0.001	0.043±0.003
S12	1.959±0.017	1.145±0.008	0.309±0.005	0.539±0.026	0.043±0.003	0.047±0.002
S13	0.758±0.023	0.669±0.022	0.189±0.011	0.442±0.033	0.053±0.001	0.088±0.001
S14	0.824±0.019	0.722±0.016	0.153±0.005	0.338±0.023	0.097±0.001	0.101±0.004
S15	0.644±0.018	0.536±0.026	0.205±0.003	0.314±0.002	0.063±0.005	0.116±0.008
S16	0.330±0.013	0.478±0.010	0.134±0.010	0.334±0.011	0.067±0.003	0.153±0.053
S17	0.764±0.010	0.548±0.012	0.246±0.035	0.353±0.034	0.058±0.001	0.096±0.001
S18	0.854±0.017	0.628±0.006	0.236±0.001	0.326±0.017	0.078±0.001	0.136±0.002
S19	0.530±0.006	0.561±0.014	0.182±0.014	0.331±0.016	0.063±0.001	0.145±0.003
S20	0.640±0.016	0.633±0.013	0.169±0.005	0.405±0.006	0.076±0.003	0.158±0.001
S21	0.543±0.020	0.455±0.023	0.143±0.036	0.295±0.004	0.086±0.001	0.134±0.002
S22	0.641±0.017	0.535±0.026	0.168±0.011	0.352±0.012	0.063±0.001	0.190±0.007
S23	0.936±0.012	0.413±0.002	0.219±0.024	0.330±0.030	0.054±0.003	0.154±0.002
S24	0.543±0.002	0.333±0.028	0.178±0.018	0.296±0.002	0.066±0.003	0.175±0.001
S25	0.537±0.012	0.552±0.034	0.151±0.024	0.362±0.004	0.046±0.003	0.155±0.003
S26	0.726±0.005	0.427±0.025	0.160±0.026	0.408±0.004	0.042±0.001	0.145±0.002
S27	0.425±0.011	0.573±0.005	0.148±0.005	0.342±0.008	0.036±0.004	0.137±0.002
S28	0.519±0.012	0.326±0.018	0.129±0.003	0.354±0.011	0.035±0.004	0.125±0.002
S29	0.337±0.023	0.420±0.013	0.151±0.008	0.322±0.007	0.046±0.001	0.157±0.001
S30	0.475±0.012	0.338±0.023	0.149±0.006	0.329±0.014	0.045±0.003	0.109±0.005
S31	0.166±0.012	0.263±0.043	0.094±0.003	0.306±0.003	0.033±0.002	0.196±0.001
S32	0.353±0.037	0.135±0.017	0.121±0.027	0.224±0.021	0.026±0.003	0.205±0.002
S33	0.531±0.010	0.257±0.021	0.133±0.027	0.275±0.012	0.035±0.003	0.195±0.003
S34	0.278±0.011	0.341±0.018	0.045±0.001	0.308±0.001	0.025±0.004	0.181±0.006
S35	0.359±0.024	0.349±0.006	0.112±0.011	0.260±0.017	0.024±0.003	0.174±0.003
S36	0.173±0.018	0.222±0.012	0.096±0.002	0.289±0.013	0.015±0.003	0.150±0.004
S37	0.236±0.036	0.369±0.027	0.013±0.001	0.250±0.016	0.025±0.002	0.182±0.006
S38	0.359±0.013	0.277±0.027	0.069±0.027	0.258±0.006	0.008±0.001	0.151±0.021
S39	0.129±0.006	0.156±0.021	0.068±0.022	0.308±0.001	0.016±0.001	0.167±0.001
S40	0.271±0.022	0.197±0.001	0.082±0.024	0.241±0.005	0.025±0.001	0.153±0.004
S41	0.241±0.006	0.226±0.018	0.052±0.005	0.205±0.001	0.024±0.004	0.165±0.004
S42	0.148±0.014	0.323±0.016	0.090±0.011	0.252±0.012	0.016±0.003	0.177±0.003
S43	0.467±0.019	0.364±0.017	0.122±0.002	0.314±0.016	0.025±0.002	0.235±0.037
S44	0.535±0.034	0.429±0.022	0.124±0.001	0.297±0.001	0.035±0.002	0.230±0.013
S45	0.252±0.033	0.480±0.021	0.124±0.001	0.315±0.001	0.035±0.004	0.308±0.005
S46	0.537±0.025	0.538±0.006	0.123±0.001	0.318±0.010	0.046±0.001	0.283±0.013
S47	0.635±0.006	0.332±0.032	0.152±0.005	0.296±0.007	0.052±0.001	0.308±0.001
S48	0.667±0.012	0.623±0.008	0.096±0.002	0.348±0.007	0.037±0.001	0.257±0.009
S49	0.813±0.001	0.731±0.028	0.103±0.001	0.322±0.003	0.046±0.004	0.292±0.005
S50	0.644±0.011	0.521±0.013	0.222±0.002	0.305±0.004	0.053±0.003	0.251±0.023
S51	0.548±0.023	0.464±0.034	0.130±0.006	0.366±0.003	0.061±0.003	0.312±0.002
S52	0.517±0.040	0.550±0.033	0.104±0.001	0.396±0.002	0.047±0.001	0.244±0.022
S53	0.633±0.012	0.630±0.017	0.087±0.003	0.354±0.010	0.053±0.004	0.220±0.010
S54	0.453±0.010	0.729±0.010	0.407±0.526	0.336±0.013	0.044±0.003	0.255±0.010

Batch No.

Echinacoside

Acteoside

Tubuloside A

Isoacteoside

Poliumoside

Geniposide

0.548±0.006

0.637±0.012

0.232±0.017

0.637±0.015

0.045±0.002

0.095±0.002

1.132±0.031

0.964±0.023

0.222±0.012

0.542±0.006

0.045±0.003

0.091±0.006

0.858±0.014

0.841±0.027

0.237±0.051

0.643±0.011

0.048±0.001

0.056±0.003

0.749±0.006

0.682±0.006

0.196±0.002

0.538±0.013

0.054±0.003

0.075±0.001

0.972±0.024

0.766±0.022

0.283±0.016

0.479±0.024

0.038±0.001

0.065±0.003

1.259±0.017

0.696±0.174

0.312±0.007

0.541±0.023

0.047±0.003

0.074±0.004

1.128±0.007

0.895±0.003

0.383±0.016

0.755±0.010

0.043±0.001

0.064±0.004

2.027±0.018

1.118±0.110

0.219±0.016

0.637±0.016

0.055±0.004

0.065±0.003

1.358±0.006

1.150±0.017

0.337±0.053

0.535±0.005

0.044±0.002

0.094±0.003

S10

0.875±0.018

1.240±0.006

0.236±0.025

0.456±0.002

0.048±0.001

0.043±0.001

S11

1.247±0.008

0.958±0.024

0.232±0.008

0.419±0.006

0.051±0.001

0.043±0.003

S12

1.959±0.017

1.145±0.008

0.309±0.005

0.539±0.026

0.043±0.003

0.047±0.002

S13

0.758±0.023

0.669±0.022

0.189±0.011

0.442±0.033

0.053±0.001

0.088±0.001

S14

0.824±0.019

0.722±0.016

0.153±0.005

0.338±0.023

0.097±0.001

0.101±0.004

S15

0.644±0.018

0.536±0.026

0.205±0.003

0.314±0.002

0.063±0.005

0.116±0.008

S16

0.330±0.013

0.478±0.010

0.134±0.010

0.334±0.011

0.067±0.003

0.153±0.053

S17

0.764±0.010

0.548±0.012

0.246±0.035

0.353±0.034

0.058±0.001

0.096±0.001

S18

0.854±0.017

0.628±0.006

0.236±0.001

0.326±0.017

0.078±0.001

0.136±0.002

S19

0.530±0.006

0.561±0.014

0.182±0.014

0.331±0.016

0.063±0.001

0.145±0.003

S20

0.640±0.016

0.633±0.013

0.169±0.005

0.405±0.006

0.076±0.003

0.158±0.001

S21

0.543±0.020

0.455±0.023

0.143±0.036

0.295±0.004

0.086±0.001

0.134±0.002

S22

0.641±0.017

0.535±0.026

0.168±0.011

0.352±0.012

0.063±0.001

0.190±0.007

S23

0.936±0.012

0.413±0.002

0.219±0.024

0.330±0.030

0.054±0.003

0.154±0.002

S24

0.543±0.002

0.333±0.028

0.178±0.018

0.296±0.002

0.066±0.003

0.175±0.001

S25

0.537±0.012

0.552±0.034

0.151±0.024

0.362±0.004

0.046±0.003

0.155±0.003

S26

0.726±0.005

0.427±0.025

0.160±0.026

0.408±0.004

0.042±0.001

0.145±0.002

S27

0.425±0.011

0.573±0.005

0.148±0.005

0.342±0.008

0.036±0.004

0.137±0.002

S28

0.519±0.012

0.326±0.018

0.129±0.003

0.354±0.011

0.035±0.004

0.125±0.002

S29

0.337±0.023

0.420±0.013

0.151±0.008

0.322±0.007

0.046±0.001

0.157±0.001

S30

0.475±0.012

0.338±0.023

0.149±0.006

0.329±0.014

0.045±0.003

0.109±0.005

S31

0.166±0.012

0.263±0.043

0.094±0.003

0.306±0.003

0.033±0.002

0.196±0.001

S32

0.353±0.037

0.135±0.017

0.121±0.027

0.224±0.021

0.026±0.003

0.205±0.002

S33

0.531±0.010

0.257±0.021

0.133±0.027

0.275±0.012

0.035±0.003

0.195±0.003

S34

0.278±0.011

0.341±0.018

0.045±0.001

0.308±0.001

0.025±0.004

0.181±0.006

S35

0.359±0.024

0.349±0.006

0.112±0.011

0.260±0.017

0.024±0.003

0.174±0.003

S36

0.173±0.018

0.222±0.012

0.096±0.002

0.289±0.013

0.015±0.003

0.150±0.004

S37

0.236±0.036

0.369±0.027

0.013±0.001

0.250±0.016

0.025±0.002

0.182±0.006

S38

0.359±0.013

0.277±0.027

0.069±0.027

0.258±0.006

0.008±0.001

0.151±0.021

S39

0.129±0.006

0.156±0.021

0.068±0.022

0.308±0.001

0.016±0.001

0.167±0.001

S40

0.271±0.022

0.197±0.001

0.082±0.024

0.241±0.005

0.025±0.001

0.153±0.004

S41

0.241±0.006

0.226±0.018

0.052±0.005

0.205±0.001

0.024±0.004

0.165±0.004

S42

0.148±0.014

0.323±0.016

0.090±0.011

0.252±0.012

0.016±0.003

0.177±0.003

S43

0.467±0.019

0.364±0.017

0.122±0.002

0.314±0.016

0.025±0.002

0.235±0.037

S44

0.535±0.034

0.429±0.022

0.124±0.001

0.297±0.001

0.035±0.002

0.230±0.013

S45

0.252±0.033

0.480±0.021

0.124±0.001

0.315±0.001

0.035±0.004

0.308±0.005

S46

0.537±0.025

0.538±0.006

0.123±0.001

0.318±0.010

0.046±0.001

0.283±0.013

S47

0.635±0.006

0.332±0.032

0.152±0.005

0.296±0.007

0.052±0.001

0.308±0.001

S48

0.667±0.012

0.623±0.008

0.096±0.002

0.348±0.007

0.037±0.001

0.257±0.009

S49

0.813±0.001

0.731±0.028

0.103±0.001

0.322±0.003

0.046±0.004

0.292±0.005

S50

0.644±0.011

0.521±0.013

0.222±0.002

0.305±0.004

0.053±0.003

0.251±0.023

S51

0.548±0.023

0.464±0.034

0.130±0.006

0.366±0.003

0.061±0.003

0.312±0.002

S52

0.517±0.040

0.550±0.033

0.104±0.001

0.396±0.002

0.047±0.001

0.244±0.022

S53

0.633±0.012

0.630±0.017

0.087±0.003

0.354±0.010

0.053±0.004

0.220±0.010

S54

0.453±0.010

0.729±0.010

0.407±0.526

0.336±0.013

0.044±0.003

0.255±0.010