药学学报

No.	Habitat	Manufacturer	Batch	Grain number of 50 g	Length /mm	Diameter /mm	Imperfection /% (w/w)	Skin color^a
Goji-1	Ningxia Zhouta	Ningxia Zhouta	GQ-210623	281	15.76 ± 3.52	5.63 ± 0.89	3.01	1
Goji-2	GQ-210630	310	15.44 ± 2.90	5.78 ± 1.02	1.75	1
Goji-3	GQ-210709	321	15.31 ± 3.51	5.53 ± 1.16	0.94	1
Goji-4	GQ-210715	353	15.42 ± 3.69	6.10 ± 1.21	1.56	1
Goji-5	GQ-210723	330	15.26 ± 3.12	5.99 ± 1.29	1.90	1
Goji-6	GQ-210730	351	15.23 ± 1.79	5.82 ± 1.11	2.56	1
Goji-7	GQ-210623	283	16.40 ± 3.24	6.18 ± 1.24	3.02	1
Goji-8	GQ-210630	321	15.72 ± 2.44	5.62 ± 1.10	2.33	1
Goji-9	GQ-210709	331	15.31 ± 2.62	5.31 ± 1.13	2.81	1
Goji-10	Ningxia Xizan	Ningxia Xizan	GQ-210703	319	14.34 ± 2.42	5.75 ± 0.98	0.98	1
Goji-11	GQ-210710	332	15.43 ± 2.41	5.45 ± 1.15	1.52	1
Goji-12	GQ-210717	408	13.87 ± 0.95	5.46 ± 0.67	1.84	1
Goji-13	GQ-210724	410	13.05 ± 1.07	6.36 ± 0.94	1.92	1
Goji-14	GQ-210731	535	12.07 ± 1.52	5.48 ± 0.66	1.36	1
Goji-15	Ningxia Yinchuan	Ningxia Yinchuan	GQ-210706	558	11.52 ± 1.06	4.18 ± 0.70	3.57	1
Goji-16	GQ-210715	343	14.06 ± 1.85	5.32 ± 1.12	2.24	1
Goji-17	Ningxia Shizuishan	Ningxia Shizuishan	GQ-210617	331	15.55 ± 2.29	5.93 ± 1.17	0.88	1
Goji-18	GQ-210705	409	12.65 ± 0.77	4.81 ± 0.92	1.49	1
Goji-19	GQ-210615	271	15.34 ± 2.34	6.54 ± 1.20	2.67	1
Goji-20	GQ-210704	440	12.36 ± 1.68	4.38 ± 0.59	2.65	1
Goji-21	Ningxia	Shanghai Kangqiao	GQ-21090701	373	14.99 ± 1.80	5.83 ± 0.55	0.92	2
Goji-22	GQ-21090702	307	14.77 ± 2.33	5.75 ± 0.66	2.56	1
Goji-23	GQ-22081801	386	14.52 ± 2.52	5.49 ± 1.06	2.17	2
Goji-24	GQ-22081802	549	12.11 ± 1.82	4.61 ± 0.63	1.82	2
Goji-25	GQ-22081803	386	14.73 ± 2.14	5.81 ± 0.69	1.75	2
Goji-26	GQ-22081804	540	12.35 ± 1.27	4.74 ± 0.39	2.46	1
Goji-27	GQ-22081805	377	14.72 ± 2.63	6.19 ± 1.09	2.00	2
Goji-28	GQ-22081806	560	12.34 ± 2.32	4.71 ± 0.84	0.87	1
Goji-29	GQ-22081807	374	14.36 ± 2.32	5.98 ± 0.69	2.57	2
Goji-30	GQ-22081808	547	12.33 ± 1.70	4.75 ± 0.71	2.10	1
Goji-31	GQ-22081809	387	14.53 ± 3.12	5.96 ± 0.86	1.02	2
Goji-32	GQ-22081810	538	12.70 ± 1.28	4.20 ± 0.64	2.64	1

No.	Habitat	Manufacturer	Batch	Grain number of 50 g	Length /mm	Diameter /mm	Imperfection /% (w/w)	Skin color^a
Goji-1	Ningxia Zhouta	Ningxia Zhouta	GQ-210623	281	15.76 ± 3.52	5.63 ± 0.89	3.01	1
Goji-2	GQ-210630	310	15.44 ± 2.90	5.78 ± 1.02	1.75	1
Goji-3	GQ-210709	321	15.31 ± 3.51	5.53 ± 1.16	0.94	1
Goji-4	GQ-210715	353	15.42 ± 3.69	6.10 ± 1.21	1.56	1
Goji-5	GQ-210723	330	15.26 ± 3.12	5.99 ± 1.29	1.90	1
Goji-6	GQ-210730	351	15.23 ± 1.79	5.82 ± 1.11	2.56	1
Goji-7	GQ-210623	283	16.40 ± 3.24	6.18 ± 1.24	3.02	1
Goji-8	GQ-210630	321	15.72 ± 2.44	5.62 ± 1.10	2.33	1
Goji-9	GQ-210709	331	15.31 ± 2.62	5.31 ± 1.13	2.81	1
Goji-10	Ningxia Xizan	Ningxia Xizan	GQ-210703	319	14.34 ± 2.42	5.75 ± 0.98	0.98	1
Goji-11	GQ-210710	332	15.43 ± 2.41	5.45 ± 1.15	1.52	1
Goji-12	GQ-210717	408	13.87 ± 0.95	5.46 ± 0.67	1.84	1
Goji-13	GQ-210724	410	13.05 ± 1.07	6.36 ± 0.94	1.92	1
Goji-14	GQ-210731	535	12.07 ± 1.52	5.48 ± 0.66	1.36	1
Goji-15	Ningxia Yinchuan	Ningxia Yinchuan	GQ-210706	558	11.52 ± 1.06	4.18 ± 0.70	3.57	1
Goji-16	GQ-210715	343	14.06 ± 1.85	5.32 ± 1.12	2.24	1
Goji-17	Ningxia Shizuishan	Ningxia Shizuishan	GQ-210617	331	15.55 ± 2.29	5.93 ± 1.17	0.88	1
Goji-18	GQ-210705	409	12.65 ± 0.77	4.81 ± 0.92	1.49	1
Goji-19	GQ-210615	271	15.34 ± 2.34	6.54 ± 1.20	2.67	1
Goji-20	GQ-210704	440	12.36 ± 1.68	4.38 ± 0.59	2.65	1
Goji-21	Ningxia	Shanghai Kangqiao	GQ-21090701	373	14.99 ± 1.80	5.83 ± 0.55	0.92	2
Goji-22	GQ-21090702	307	14.77 ± 2.33	5.75 ± 0.66	2.56	1
Goji-23	GQ-22081801	386	14.52 ± 2.52	5.49 ± 1.06	2.17	2
Goji-24	GQ-22081802	549	12.11 ± 1.82	4.61 ± 0.63	1.82	2
Goji-25	GQ-22081803	386	14.73 ± 2.14	5.81 ± 0.69	1.75	2
Goji-26	GQ-22081804	540	12.35 ± 1.27	4.74 ± 0.39	2.46	1
Goji-27	GQ-22081805	377	14.72 ± 2.63	6.19 ± 1.09	2.00	2
Goji-28	GQ-22081806	560	12.34 ± 2.32	4.71 ± 0.84	0.87	1
Goji-29	GQ-22081807	374	14.36 ± 2.32	5.98 ± 0.69	2.57	2
Goji-30	GQ-22081808	547	12.33 ± 1.70	4.75 ± 0.71	2.10	1
Goji-31	GQ-22081809	387	14.53 ± 3.12	5.96 ± 0.86	1.02	2
Goji-32	GQ-22081810	538	12.70 ± 1.28	4.20 ± 0.64	2.64	1

Item	Bright-red	Dark-red	Large size	Small size	First grade	Second grade
n	13	40	21	32	6	47
Length/mm	14.45 ± 2.29	14.60 ± 2.51	17.40 ± 0.92	12.70 ± 0.61	16.77 ± 0.38	14.28 ± 2.44
Diameter/mm	5.78 ± 0.54	5.56 ± 0.86	6.38 ± 0.45	5.11 ± 0.52	6.15 ± 0.43	5.55 ± 0.81
Moisture/%	7.37 ± 0.77^****	9.38 ± 1.07	8.96 ± 1.38	8.83 ± 1.30	7.26 ± 0.52^∆∆∆	9.09 ± 1.52
Ash/%	4.23 ± 0.19	4.24 ± 0.26	4.23 ± 0.25	4.24 ± 0.24	4.12 ± 0.12	4.25 ± 0.25
Water-soluble extractives/%	68.51 ± 3.17^*	64.67 ± 5.12	66.72 ± 4.88	64.88 ± 4.97	69.99 ± 3.70^∆	65.05 ± 4.86
Volatile ether extractives/%	0.62 ± 0.08	0.58 ± 0.09	0.58 ± 0.09	0.59 ± 0.09	0.64 ± 0.07	0.58 ± 0.09
LBP/%	3.02 ± 0.52^*	2.50 ± 0.65	2.68 ± 0.63	2.59 ± 0.68	2.98 ± 0.55	2.58 ± 0.66
Betaine/%	0.75 ± 0.16	0.85 ± 0.17	0.73 ± 0.13^##	0.88 ± 0.17	0.64 ± 0.11^∆∆	0.85 ± 0.16
AA-2βG/%	1.23 ± 0.14^****	0.72 ± 0.24	0.77 ± 0.33	0.89 ± 0.29	1.22 ± 0.18^∆∆	0.80 ± 0.29
ZD/%	0.27 ± 0.05^***	0.20 ± 0.06	0.23 ± 0.06	0.20 ± 0.07	0.28 ± 0.05^∆∆	0.20 ± 0.06

Item	Bright-red	Dark-red	Large size	Small size	First grade	Second grade
n	13	40	21	32	6	47
Length/mm	14.45 ± 2.29	14.60 ± 2.51	17.40 ± 0.92	12.70 ± 0.61	16.77 ± 0.38	14.28 ± 2.44
Diameter/mm	5.78 ± 0.54	5.56 ± 0.86	6.38 ± 0.45	5.11 ± 0.52	6.15 ± 0.43	5.55 ± 0.81
Moisture/%	7.37 ± 0.77^****	9.38 ± 1.07	8.96 ± 1.38	8.83 ± 1.30	7.26 ± 0.52^∆∆∆	9.09 ± 1.52
Ash/%	4.23 ± 0.19	4.24 ± 0.26	4.23 ± 0.25	4.24 ± 0.24	4.12 ± 0.12	4.25 ± 0.25
Water-soluble extractives/%	68.51 ± 3.17^*	64.67 ± 5.12	66.72 ± 4.88	64.88 ± 4.97	69.99 ± 3.70^∆	65.05 ± 4.86
Volatile ether extractives/%	0.62 ± 0.08	0.58 ± 0.09	0.58 ± 0.09	0.59 ± 0.09	0.64 ± 0.07	0.58 ± 0.09
LBP/%	3.02 ± 0.52^*	2.50 ± 0.65	2.68 ± 0.63	2.59 ± 0.68	2.98 ± 0.55	2.58 ± 0.66
Betaine/%	0.75 ± 0.16	0.85 ± 0.17	0.73 ± 0.13^##	0.88 ± 0.17	0.64 ± 0.11^∆∆	0.85 ± 0.16
AA-2βG/%	1.23 ± 0.14^****	0.72 ± 0.24	0.77 ± 0.33	0.89 ± 0.29	1.22 ± 0.18^∆∆	0.80 ± 0.29
ZD/%	0.27 ± 0.05^***	0.20 ± 0.06	0.23 ± 0.06	0.20 ± 0.07	0.28 ± 0.05^∆∆	0.20 ± 0.06

Item	Length	Diameter	Skin color	Moisture	Ash	Water- soluble extractives	Volatile ether extractives	LBP	Betaine	AA-2βG	ZD
Length	1
Diameter	0.814^**	1
Skin color	-0.039	0.121	1
Moisture	0.078	-0.036	-0.669^**	1
Ash	-0.046	-0.154	-0.079	-0.090	1
Water-soluble extractives	0.199	0.179	0.343^*	-0.487^**	-0.099	1
Volatile ether extractives	-0.059	-0.108	0.225	-0.365^**	0.035	0.159	1
LBP	-0.067	-0.095	0.317^*	-0.104	0.038	0.006	0.124	1
Betaine	-0.371^**	-0.325^*	-0.236	0.125	0.013	-0.135	0.138	-0.005	1
AA-2βG	-0.305^*	-0.114	0.719^**	-0.414^**	-0.183	0.250	0.258	0.175	-0.033	1
ZD	0.083	0.074	0.496^**	-0.334^*	-0.053	0.159	-0.243	0.375^**	-0.384^**	0.469^**	1

Item	Length	Diameter	Skin color	Moisture	Ash	Water- soluble extractives	Volatile ether extractives	LBP	Betaine	AA-2βG	ZD
Length	1
Diameter	0.814^**	1
Skin color	-0.039	0.121	1
Moisture	0.078	-0.036	-0.669^**	1
Ash	-0.046	-0.154	-0.079	-0.090	1
Water-soluble extractives	0.199	0.179	0.343^*	-0.487^**	-0.099	1
Volatile ether extractives	-0.059	-0.108	0.225	-0.365^**	0.035	0.159	1
LBP	-0.067	-0.095	0.317^*	-0.104	0.038	0.006	0.124	1
Betaine	-0.371^**	-0.325^*	-0.236	0.125	0.013	-0.135	0.138	-0.005	1
AA-2βG	-0.305^*	-0.114	0.719^**	-0.414^**	-0.183	0.250	0.258	0.175	-0.033	1
ZD	0.083	0.074	0.496^**	-0.334^*	-0.053	0.159	-0.243	0.375^**	-0.384^**	0.469^**	1

Item	Grade
General information	Origin	Dried ripe fruit of Lycium barbarum L. (Fam. Solanaceae)
Wild/cultivated	Cultivated
Processing	Harvested in summer and fall when the fruit is red, dried in hot air, or aired until the skin is wrinkled, dried in the sun, then removing the pedicel
Morphological features	Shape	Nearly fusiform or elliptical
Surface feature	Stylar scars apically with small protuberant scars, basally with white fruiting pedicel scars
Texture	Pericarp is soft and externally roughly wrinkled; Sarcocarp is pulpy, soft and tender
Odor and taste	Slight; sweet
Seeds	20 to 50 seeds; brown-yellow; kidney-shaped and flat; 1.5-1.9 mm in length, 1-1.7 mm in diameter
Skin color	Bright-red	Dark-red
Grain number of 50 g	≤ 280	≤ 560
Length	≥ 16.00 mm	6.00-16.00 mm
Diameter	≥ 6.00 mm	3.00-6.00 mm
Imperfection	≤ 1.00%	≤ 3.00%
Test index	Moisture	≤ 8.00%	≤ 13.00%
Total ash	≤ 5.00%
Water-soluble extractives	≥ 70.00%	≥ 55.00%
Marker components contents	LBP	≥ 3.00%	≥ 1.80%
AA-2βG	≥ 1.00%	≥ 0.30%
ZD	≥ 0.25%	≥ 0.10%
Betaine	≥ 0.50%

Item	Grade
General information	Origin	Dried ripe fruit of Lycium barbarum L. (Fam. Solanaceae)
Wild/cultivated	Cultivated
Processing	Harvested in summer and fall when the fruit is red, dried in hot air, or aired until the skin is wrinkled, dried in the sun, then removing the pedicel
Morphological features	Shape	Nearly fusiform or elliptical
Surface feature	Stylar scars apically with small protuberant scars, basally with white fruiting pedicel scars
Texture	Pericarp is soft and externally roughly wrinkled; Sarcocarp is pulpy, soft and tender
Odor and taste	Slight; sweet
Seeds	20 to 50 seeds; brown-yellow; kidney-shaped and flat; 1.5-1.9 mm in length, 1-1.7 mm in diameter
Skin color	Bright-red	Dark-red
Grain number of 50 g	≤ 280	≤ 560
Length	≥ 16.00 mm	6.00-16.00 mm
Diameter	≥ 6.00 mm	3.00-6.00 mm
Imperfection	≤ 1.00%	≤ 3.00%
Test index	Moisture	≤ 8.00%	≤ 13.00%
Total ash	≤ 5.00%
Water-soluble extractives	≥ 70.00%	≥ 55.00%
Marker components contents	LBP	≥ 3.00%	≥ 1.80%
AA-2βG	≥ 1.00%	≥ 0.30%
ZD	≥ 0.25%	≥ 0.10%
Betaine	≥ 0.50%

宁夏道地药材枸杞子等级质量标准研究

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余钟莲 ¹ , 李薛萍 ²^,³ , 杨莉 ⁴ , 王峥涛 ⁴ , 刘文静 ⁵ , 王瑞 ¹^,^* , 石燕红 ²^,³^,^*

药学学报 | 研究论文 2024,59(5): 1399-1407

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药学学报 | 研究论文 2024, 59(5): 1399-1407

宁夏道地药材枸杞子等级质量标准研究

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余钟莲¹, 李薛萍²^,³, 杨莉⁴, 王峥涛⁴, 刘文静⁵, 王瑞¹^,^*, 石燕红²^,³^,^*

作者信息

1.上海中医药大学中药学院, 上海 201203

2.上海中医药大学中医药国际标准化研究所, 上海 201203

3.上海市中医药国际标准化研究院, 上海 201203

4.上海中医药大学中药研究所, 中药标准化教育部重点实验室, 上海 201203

5.上海市浦东新区公利医院, 上海 200135

通讯作者:

^*王瑞, E-mail: ellewang@163.com;

石燕红, E-mail: shiyhtcm@shutcm.edu.cn

Grade quality standard development of Lycium barbarum fruits from Ningxia genuine producing area

Zhong-lian YU¹, Xue-ping LI²^,³, Li YANG⁴, Zheng-tao WANG⁴, Wen-jing LIU⁵, Rui WANG¹^,^*, Yan-hong SHI²^,³^,^*

Affiliations

1. School of Pharmacy, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China

2. Institute of International Standardization for Traditional Chinese Medicine, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China

3. Shanghai Academy of International Standardization for Traditional Chinese Medicine, Shanghai 201203, China

4. The MOE Key Laboratory of Standardization of Chinese Medicines, Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China

5. Shanghai Pudong New Area Gongli Hospital, Shanghai 200135, China

出版时间: 2024-05-12 doi: 10.16438/j.0513-4870.2023-1346

文章导航

摘要

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基于传统性状鉴别结合现代中药分析手段的综合评价模式用于宁夏道地药材枸杞子等级划分关键指标的辨识和等级质量标准的建立。本草考证和市场调查指导下, 将粒径大小、表皮颜色和不完善粒作为外在性状指标; 聚焦枸杞子品质评价的全面性和有效性, 在水分、灰分、水溶性浸出物、枸杞多糖(Lycium barbarum polysaccharide, LBP) 和甜菜碱等药典规定指标的基础上, 增加枸杞酸(2-O-β-D-glucopyranosyl-L-ascorbic acid, AA-2βG)、玉米黄质双棕榈酸酯(zeaxanthin dipalmitate, ZD) 和挥发性醚浸出物为内在质量指标。并通过t检验、相关性分析和主成分分析等数理统计方法, 考察不同等级枸杞子外观性状与内在质量的关联, 从而进行质量等级的划分和标准的制定, 最后从体外细胞水平比较不同等级枸杞子提取物的活性差异。结果表明, 枸杞子主要以“粒大色红”为佳; 除甜菜碱外, 其余指标成分均在表皮颜色鲜红和一等枸杞子中相对偏高; 表皮颜色和水分、水溶性浸出物、LBP、AA-2βG和ZD含量之间存在显著相关。综合研究结果和市场流通情况, 本研究以枸杞子的粒径大小和表皮颜色为基础, 同时引入LBP、AA-2βG、ZD、水溶性浸出物和水分等多指标进一步指导等级划分, 建立了外观性状和内在质量关键指标相结合的宁夏道地药材枸杞子等级质量标准, 体外细胞活性也初步证实了一等枸杞子具有更为显著的“滋补肝肾”活性, 这为枸杞子的质量控制和优质优价的实现提供了实验依据。

关键词

枸杞子 / 道地产区 / 外观性状 / 内在质量 / 等级质量标准

Abstract

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An integrated evaluation model based on the combination of traditional trait identification and modern chemical analysis was used for the identification of key indexes of grade classification and the establishment of grade quality standard of Lycium barbarum fruits (LBF) from Ningxia genuine producing area. Under the guidance of herbal examination and market survey, particle size, skin color and imperfection were taken as the external trait indicators; focusing on the comprehensiveness and validity of the quality evaluation, 2-O-β-D-glucopyranosyl-L-ascorbic acid (AA-2βG), zeaxanthin dipalmitate (ZD) and volatile ether extractives were used as important parameters involving in quality evaluation in addition to the pharmacopoeia test items and determination indicators such as moisture, ash, water-soluble extractives, Lycium barbarum polysaccharide (LBP) and betaine. The quality differences between different traits and grades of LBF as well as the relevance between character and quality were further investigated by mathematical and statistical means such as t-test analysis, correlation analysis and principal component analysis (PCA). Furthermore, the activities of extractives from different grades of LBF were compared at cellular level. The results showed that LBF were mainly preferred for large and red ones; except for betaine, the other index components were relatively high (moisture and ash were low) in the first-grade and samples with bright-red skin color. Besides, there was a significant correlation between skin color and moisture, water-soluble extractives, LBP, AA-2βG and ZD contents. Considering the results of the study and the market situation, the present study took the grain size and skin color of LBF as the core of evaluation, and at the same time introduced the multi-indicator components including LBP, AA-2βG, ZD, water-soluble extractives and moisture to further guide the grading, and established the quality standard of LBF grades combining the trait indexes and the chemical composition. More importantly, in vitro cell models both preliminarily confirmed that the first-grade LBF played a more significant "nourishing liver and kidney" effect, which provided an experimental basis for the quality control of LBF and promoted the realization of high quality and good price.

Key words

Lycium barbarum fruit / genuine producing area / appearance trait / inner quality marker / grade quality standard

引用本文

余钟莲, 李薛萍, 杨莉, 王峥涛, 刘文静, 王瑞, 石燕红. 宁夏道地药材枸杞子等级质量标准研究. 药学学报, 2024 , 59 (5) : 1399 -1407 . DOI: 10.16438/j.0513-4870.2023-1346

Zhong-lian YU, Xue-ping LI, Li YANG, Zheng-tao WANG, Wen-jing LIU, Rui WANG, Yan-hong SHI. Grade quality standard development of Lycium barbarum fruits from Ningxia genuine producing area[J]. Acta Pharmaceutica Sinica, 2024 , 59 (5) : 1399 -1407 . DOI: 10.16438/j.0513-4870.2023-1346

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中药材的等级质量标准是衡量中药质量优劣的重要依据, 对保障临床用药安全有效、合理配置中药资源至关重要。中药材等级的划分历史悠久, 性状和产地是其主要的评价指标。《七十六种药材商品规格标准》是现行的主要标准; 近年来, 中华中医药学会进一步优化并发布了200多种常用中药材的商品规格等级标准。随着中药现代化进程的加快, 以及中药材饮片市场的产业发展和需求变化, 现行中药材商品规格等级标准并不能完全准确地反映药材的质量优劣情况, 且药材的外观性状与内在品质没有密切关联甚至可能相互矛盾, 如一等制远志中远志𠮿酮Ⅲ等三种成分的含量均低于二等品^[1]。因此需要不断完善中药材等级标准以适应实际需求, 尤其是枸杞子和人参等需求量大、应用广泛的大宗类药材, 应引导优质优价, 以提高中药材及其饮片质量, 促进中医药事业的高质量发展^[2]。

枸杞子为茄科植物宁夏枸杞(Lycium bararum L.) 的干燥成熟果实, 具有滋补肝肾、益精明目的功效, 为药食同源佳品^[3]。枸杞子广泛分布于我国西北部, 如宁夏、青海、甘肃、新疆和内蒙古等地, 其中宁夏为枸杞子的道地产区。据本草考证和现代文献研究发现, 产地来源、采收时间、加工方式和运输储存等因素都会导致枸杞子的外观性状和内在质量存在显著差异^{[4, 5]}。1977年版《中华人民共和国药典》首次规定宁夏枸杞(Lycium bararum L.) 为枸杞子的唯一基源, 且“以粒大、色红、肉厚、质柔润、籽少、味甜者为佳”^[6]。目前, 枸杞子等级标准的研究内容较少且仅聚焦于性状特征, 如《七十六种药材商品规格标准》基于产地、果皮颜色、糖质、50 g粒度等指标进行划分^[7]; 《中药材商品规格等级—枸杞子》则仅以粒度和不完善粒为主要区别点^[8]; 王丹等^[9]通过面积值、重量值及均匀度初步建立枸杞子商品等级标准。然而, 现有的划分标准均缺乏系统科学的内在质量评价参数, 在药材“辨状论质”的研究基础上, 应引入能体现中药药效的内在品质指标及测定方法, 进一步完善相关标准。

枸杞子成分丰富多样, 主要含有枸杞多糖(Lycium barbarum polysaccharides, LBP)、类胡萝卜素、生物碱、黄酮多酚等, 具有调节免疫、抗氧化、抗衰老、降血脂血糖、抗肿瘤等多种作用^[10]。2020版中国药典将LBP和甜菜碱作为枸杞子的含量测定项, 仅依据以上两个指标成分无法全面表征枸杞子多成分多功效的属性特点。因此, 亟需寻找其他含量丰富、专属性较强、药理作用显著的指标性成分以提升枸杞子的品质研究。枸杞酸(2-O-β-D-glucopyranosyl-L-ascorbic acid, AA-2βG) 是一种稳定的维生素C衍生物, 其在枸杞子中的含量可高达1.33%, 研究报道称其可以发挥降糖, 调节肠道微生物群以及抑制HeLa细胞增殖等作用^[11-14]。类胡萝卜素是一类脂溶性活性成分, 也是枸杞子主要的内在呈色物质, 玉米黄质双棕榈酸酯(zeaxanthin dipalmitate, ZD) 是成熟枸杞子中最主要的类胡萝卜素成分, 含量可达70%以上^[15]。研究表明ZD具有清肝明目的功效, 对酒精性脂肪肝以及乙肝等肝损伤、色素性视网膜炎等眼部疾病具有缓解和治疗作用^[16-18]。前期课题组研究发现, 枸杞子脂溶性成分, 尤其是类胡萝卜素类成分, 具有显著的5α-还原酶抑制作用, 对良性前列腺增生有一定治疗作用, 可能与枸杞子滋补肝肾的传统功效相关^[19]。因此, 在现有质量标准的基础上, 本研究增加AA-2βG、ZD和挥发性醚浸出物作为药材内在质量控制指标成分, 以完善枸杞子的质量评价与等级标准划分。药效是中药质量评价的重要指标, 也是验证中药质量等级标准合理性和科学性的重要依据, 本研究进一步基于枸杞子“滋补肝肾”的传统功效, 分别建立人肝癌细胞HepG2模型和脂多糖(lipopolysaccharide, LPS) 诱导的人肾小管上皮细胞HK-2损伤模型, 从体外细胞水平快速比较不同等级枸杞子的活性差异, 为等级标准的建立提供支撑依据。

综上所述, 本研究结合传统中药分级策略与现代中药标准化研究方法, 探索枸杞子的外观性状和内在质量之间的联系, 挖掘能体现优质枸杞子品质特征的等级划分关键指标(群), 建立科学适用的枸杞子质量分级体系, 并通过体外细胞水平来进行不同等级枸杞子提取物的活性比较与验证, 为枸杞子质量标准的提升、等级质量标准的建立和优质优价的实现提供技术和标准支撑。

材料与方法

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仪器 Agilent 1260型高效液相色谱仪(美国Agilent公司); ACQUITY UPC²超高效合相色谱(美国Waters公司); WFJ-7200型可见分光光度计仪(上海尤尼柯仪器有限公司); HWS-24恒温水浴锅(上海诚献仪器设备有限公司); Milli-Q Advantage型超纯水系统(美国Millipore公司); BT25S型电子分析天平(德国Sartorins公司); KQ-250DB数控超声波清洗器(昆山市超声仪器有限公司); 数显游标卡尺(北京能克工程有限公司); Thermo HERH CELL 150培养箱和Varioskan Flash全波长酶标仪(美国Thermo Fisher公司); Centrifuge 5424 R离心机(德国Eppendorf公司)。

试剂和细胞系 甜菜碱(批号110894-201604; 纯度≥ 99%)、无水葡萄糖(批号110833-201908) 购于中国食品药品检定研究院; 枸杞酸(批号8030; 纯度≥ 98%) 购于上海诗丹德标准技术服务公司; 玉米黄质双棕榈酸酯(批号14, UV ≥ 95%) 购于法国Extrasynthese公司; 色谱级试剂甲醇和乙腈, 分析纯试剂甲醇、乙醇、盐酸、氨水、正己烷、乙酸乙酯和氯化胆碱、丙二酸等试剂购于上海国药集团化学试剂有限公司; 高纯度CO₂ (纯度≥ 99.999%) 由上海氯闵气体有限公司提供。DMEM培养基(批号MA0213-Jan-18I)、胰酶(批号MA0232-Mar-30I1)、双抗(批号MA0110-Mar-24I) 和CCK-8 (批号MA0218-Jun-15I) 等试剂购于上海美仑生物公司; 胎牛血清(批号10099-141) 购于美国Gibco公司; HepG2细胞和HK-2细胞购于中国科学院上海生命科学院细胞资源中心, 均接种于含10%胎牛血清, 1%双抗的DMEM培养基中, 置于含5% CO₂的37 ℃恒温培养箱中培养。

样品目前共收集枸杞子样品32批, 其中20批样品采集于宁夏生产基地, 12批样品收集于上海康桥中药饮片有限公司, 均来自于宁夏道地产区。上海市中医药国际标准化研究院吴立宏研究员鉴定为茄科植物宁夏枸杞Lycium barbarum L.的干燥成熟果实, 标本保存在上海市中医药国际标准化研究院。样品来源及批号见表 1。

性状指标测定和等级划分 为了更为直观地反映宁夏道地药材枸杞子外观性状特点, 本研究基于本草考证和市场调查情况, 选择枸杞子50 g粒度、单粒长度和直径以及表皮颜色作为外观性状评价指标。采用圆锥四分法测定每批样品的50 g粒度, 同时挑选破碎粒、未成熟粒和尚有使用价值的油果, 计算不完善粒质量分数, 以上进行双试验取平均值; 每批随机挑选20粒枸杞子, 用游标卡尺测定长度(顶端至基部) 和直径(腹部最宽处)。表皮颜色通过三位志愿者的感官评价, 划分为表皮颜色暗红和鲜红两类(分别用数字1、2表示)。基于2020年版中国药典枸杞子项下的性状描述, 并以测量数据的前20%作为一等和统货界限, 数值均取较为接近的整数值, 制定一等和统货枸杞子的分级标准。基于分级标准, 在32批药材中挑选不同性状和等级的枸杞子进行后续实验。

检查项测定 水分按照2020年版中国药典通则0832水分测定法项下第二法(温度80 ℃) 测定; 灰分按照2020年版中国药典通则2302灰分测定法项下总灰分测定法测定。

浸出物测定 水溶性浸出物和挥发性醚浸出物分别按照2020年版中国药典通则2201项下的热浸法和挥发性醚浸出物测定法测定。

多指标含量测定 LBP含量依据2020年版中国药典枸杞子项下所述方法测定; 甜菜碱、AA-2βG和ZD分别按照前期建立的方法测定^[20-22]。

外观性状与内在质量的关联性分析 采用SPSS Statistics 21软件对枸杞子的内在质量指标数据按照性状和等级分组情况进行t检验分析, 并将外观性状数据和质量指标数据进行Person相关性分析。运用Simca 13.0软件, 基于表皮颜色的差异对标准化处理后的质量指标数据进行主成分分析(principal component analysis, PCA) 和正交偏最小二乘法判别分析(orthogonal partial least squares-discriminant analysis, OPLS-DA)。

提取物制备 称取研碎的枸杞子(一等和统货各3批) 置于烧瓶中, 分别加入9倍量纯水和石油醚浸泡30 min后回流1 h, 药渣再加7倍量纯水回流1 h, 过滤, 合并滤液, 减压浓缩成浸膏后冻干成粉末即得枸杞子水溶性和醚溶性提取物。称取适量提取物, DMSO溶解配成质量浓度为100 mg·mL^-1的母液, 实验前用培养基稀释到给药浓度, 过0.22 μm微孔滤膜除菌。

HK-2细胞保护活性评价 参考相关方法^[23]。基于CCK-8试剂检测不同浓度的枸杞子水溶性和醚溶性提取液(5、12.5、25、50、100 μg·mL^-1) 对HK-2细胞活力的影响, 以筛选合适的活性评价浓度。然后将处于对数生长期的HK-2细胞以10⁴个/孔(100 μL) 的密度均匀接种在96孔板中, 每组6个复孔, 培养24 h后, 模型组和给药组加入10 μg·mL^-1 LPS对细胞进行诱导损伤, 同时给药组加入相应药物共同培养, 对照组加入含1‰ DMSO的培养基, 24 h后更换为100 μL含有10% CCK-8的培养基培养30 min, 使用酶标仪检测A_{450 nm}。

HepG2细胞抑制活性评价 参考相关方法^[24]。将处于对数生长期的HepG2细胞以10⁴个/孔(100 μL) 的密度均匀接种在96孔板中, 每组6个复孔。培养24 h后, 给药组加入相应药物, 对照组加入含1‰ DMSO的培养基, 继续培养24 h后更换为含10% CCK-8的培养基培养1 h, 使用酶标仪检测A_{450 nm}。

结果

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1 外观性状等级划分

由表 1可知, 32批枸杞子的50 g粒度范围为271~560, 单粒枸杞子的长度范围为9.37~22.52 mm, 直径范围3.35~8.94 mm, 不完善粒范围为0.87%~3.57%, 表皮颜色鲜红和暗红的枸杞子各有6批和26批。同一批枸杞子普遍存在大小不均的现象, 50 g粒度无法全面合理表征枸杞子的大小情况, 因此将单粒枸杞子的长度和直径作为粒径大小的测量指标。基于上述划分方法, 最终将长度≥ 16.00 mm, 直径≥ 6.00 mm的枸杞子归为大粒径; 长度范围为6.00~16.00 mm, 直径范围为3.00~6.00 mm为小粒径。同时符合表皮颜色鲜红和大粒径的枸杞子为一等, 其余为统货。同时参考现有标准, 一等枸杞子的不完善粒要求≤ 1.00%, 统货枸杞子≤ 3.00%。

按照上述标准, 将32批枸杞子以单粒长度直径和表皮颜色作等级划分依据, 共划分为53批, 其中一等6批, 统货47批, 相关性状数据见表 2。53批样本按照粒径大小可以划分为21批大粒径和32批小粒径枸杞子; 按照表皮颜色差异可以分为13批鲜红和40批暗红的枸杞子。以外观性状初步划分的不同等级枸杞子药材将用于后续内在质量的综合评价分析。

2 检查项

53批枸杞子测定结果表明(表 2), 各批宁夏枸杞子样品水分≤ 13.00%, 总灰分≤ 5.00%, 均符合2020版中国药典要求。

3 浸出物

53批枸杞子测定结果表明(表 2), 各批宁夏枸杞子样品水溶性浸出物范围为55.29%~75.99%, 符合2020版中国药典要求; 挥发性醚浸出物范围为0.46%~0.77%。

4 多指标含量测定

53批枸杞子测定结果表明(表 2), LBP的含量范围为0.78%~4.02%, 其中4批枸杞子(Goji-5-2、Goji-6-1、Goji-7-2、Goji-19-2) 中LBP含量低于药典要求的1.8%。甜菜碱的含量范围为0.53%~1.34%, 符合2020版中国药典要求。AA-2βG的含量范围为0.30%~1.43%; ZD的含量范围为0.07%~0.35%。

5 外观性状与内在质量的关联性分析

t检验分析结果如表 2所示。LBP、AA-2βG、ZD、水溶性浸出物和挥发性醚浸出物的整体含量均在一等枸杞子和表皮颜色鲜红的样本中相对更高, 且水分和灰分在这两类样本中相对更低, 即一等和表皮颜色鲜红的枸杞子质量相对更好。此外, 不同颜色的枸杞子在水分、水溶性浸出物、LBP、AA-2βG和ZD含量中均呈现显著差异性。然而, 甜菜碱在统货、表皮颜色暗红和小粒径样本中呈现相对更高的含量, 与传统认为的优质枸杞子特征相反。除甜菜碱之外的指标成分在大粒径和小粒径枸杞子之间均不存在显著的差异, 但AA-2βG在小粒径枸杞子中整体含量更高。灰分和挥发性醚浸出物的含量在不同等级和性状样本中不存在明显差异。

相关性分析结果(表 3) 与t检验基本一致, 枸杞子的表皮颜色和水分、水溶性浸出物、LBP、AA-2βG和ZD均都存在显著性相关, 颜色越鲜红, 水分含量越低, 其他成分含量越高, 枸杞子质量越好。然而AA-2βG和甜菜碱含量与粒径大小指标之间均呈现负相关, 这与传统认为的枸杞子“粒大色红者为佳”相悖; 此外, 灰分和挥发性醚浸出物与外观性状之间不存在显著关联性。

进一步的PCA得分图(图 1A) 和OPLS-DA得分图(图 1C) 结果均表明, 基于本研究的8个质量指标成分基本可以实现表皮颜色鲜红和暗红的枸杞子的区分。载荷图(图 1B) 和VIP图(图 1D) 显示水分、AA-2βG和ZD是主要的差异贡献成分(VIP > 1), 这表明以上三个成分可以作为枸杞子质量评价的重要指标。

综合以上分析结果, 枸杞子表皮颜色和水分、AA-2βG、LBP、ZD、水溶性浸出物均存在显著相关且表现为“色红者佳”, 而粒径大小与甜菜碱、AA-2βG含量表现为负相关, 灰分和挥发性醚浸出物与外观性状无明显关联性, 且挥发性醚浸出物操作复杂, 毒性溶剂使用量大, 在大批量样本检测中缺乏一定的实操性。因此, 本研究根据2020版中国药典要求将甜菜碱和灰分仅作为枸杞子的质控成分, 不参与等级划分; 挥发性醚浸出物测定不作要求, AA-2βG、LBP、ZD、水分和水溶性浸出物共同作为枸杞子的质量分级指标。

6 枸杞子药材等级标准的制定

由于市场流通中50 g粒度是等级划分的主要依据, 因此仍将粒径大小作为性状划分指标, 同时增加表皮颜色作为外观性状区别项。结合前期研究结论, 在符合2020版中国药典的基础上, 以测定样本数据(从优到劣) 的前20%为界限划定一等枸杞子的含量界限, 其余归为统货, 由此制定了新的枸杞子药材等级分级标准, 具体分级方法见表 4。

7 不同等级枸杞子活性差异比较

细胞毒性结果显示枸杞子水提取物和石油醚提取物在5~100 μg·mL^-1范围内对HK-2细胞的活力无显著影响(图 2A), 因此将100 μg·mL^-1作为活性评价的给药浓度。基于LPS成功诱导HK-2细胞损伤后, 各批次枸杞子醚溶性浸出物均能够显著改善HK-2细胞活力, 且一等枸杞子的活性显著优于统货枸杞子(P < 0.01, 图 2B)。相较于醚溶性浸出物, 枸杞子的水溶性浸出物具有更为显著的抑制HepG2细胞增殖的作用, 且一等枸杞子的抑制活性显著高于统货枸杞子(P < 0.05, 图 2C)。

讨论

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本研究基于外观性状和内在质量为核心的“质-量”双标综合评价策略, 建立了宁夏道地药材枸杞子的等级质量标准^[25]。相较于现有的单一外观评价模式, 本研究以传统经验鉴别为核心, 找寻与外观性状紧密相关的内在指标成分来进一步评价药材质量, 同时基于课题组前期研究内容, 在药典基础上增加活性显著的关键指标成分, 以完善中药材质量评价缺乏整体性与专属性的关键问题。相较于现有的枸杞子等级标准研究成果, 本研究深入挖掘了ZD、AA-2βG和LBP等多个与枸杞子的表皮颜色高度相关的指标成分, 进一步阐述了枸杞子“辨状论质”的科学内涵。

枸杞子作为一种果实类中药材, 多以直径、单位质量内个体数、饱满度、色泽、均匀度、破碎率、含杂率和净度等指标划分等级^[26]。枸杞子的传统评价中, 在对果肉厚度、质地、种子数和甜度等指标进行评价的过程中会不可避免地对样品进行破坏, 既不利于相关研究的后续开展, 也为药材的便捷交易带来一定阻碍。因此, 本研究最终选择粒径大小和表皮颜色作为枸杞子主要的性状评价指标, 并增加不完善粒的计算进一步控制药材的质量。

大小是中药材质量判断的直观指标。枸杞子的本草著作和市场流通中均以“粒大者为佳”。本研究收集的样品中, 尤其在实地采集的枸杞子中, 普遍发现同一批样本中存在大小分布不均的现象, 传统的粒度划分并不能真实反映枸杞子的大小情况, 因此本研究主要以单粒枸杞子的长度和直径作为大小划分依据。研究结果表明枸杞子的粒径大小与甜菜碱和AA-2βG呈显著负相关, 可能与其生长期的含量变化规律有关^[27], 后期还需进一步验证探索。多数指标成分与粒径大小不存在显著的关联性, 但进一步考虑到市场“以大为美”的需求, 仍将大小作为枸杞子的划分依据。在等级划分过程中, 同时将50 g粒度和单粒大小作为划分依据, 以满足不同样品情况的评价需求。

色泽作为性状鉴别中另一个直观的指标, 与中药材内在质量有着密切关联, 品种、产地、采收、加工炮制、贮藏等因素都可能影响中药材的颜色。本研究结果表明, 枸杞子的表皮颜色与内在质量之间具有显著相关性, 进一步基于文献研究证明ZD、AA-2βG、LBP、水分的含量与枸杞子的表皮颜色存在直接或间接的联系。类胡萝卜素是枸杞子主要的内在呈色物质^[15], 文献^[28]报道其含量与枸杞子的比色数据(Lab) 之间存在高度相关性; 枸杞酸等维生素C衍生物也被证明通过抑制酪氨酸酶活性来控制水果蔬菜的酶褐变从而发挥显著的护色作用^[29]; 水分和LBP与枸杞子的“走油变色”相关^[30]。因此, 基于枸杞子的表皮颜色一定程度上可以快速准确地反映药材质量。

枸杞子药材产地、品系较多, 由此导致性状差异明显, 无法统一量化界定^[31], 故本研究主要以道地产区宁夏的枸杞子为研究对象进行等级划分。后期也将继续收集其他主产区如新疆、甘肃、青海和内蒙古等地的枸杞子, 为枸杞子的等级划分及性状和有效成分含量之间的关联性提供更加全面的信息。

本研究参考相关较为成熟的中药行业标准, 以多维度的实验数据为基础, 设定20%的比例进行枸杞子样本的等级划分。相较于需要将所有指标进行数字化处理的基于权重的综合评价模式, 该方法可以真实反映样本的性状和含量情况, 满足市场快速简单划分的需求。此外, 与聚类分析相比, 该方法计算方便、结果明确, 而聚类分析算法众多, 基于不同的聚类目的和具体应用会得到不同的聚类结果, 其结果的可靠性有待商榷。

本研究基于枸杞子“滋补肝肾”的传统功效, 分别使用不同等级的枸杞子水溶性和醚溶性提取物处理HepG2细胞和LPS诱导损伤的HK-2细胞, 并通过CCK-8法检测细胞的活性变化, 结果均表明一等枸杞子具有更为显著的药理活性, 为验证枸杞子质量等级标准的合理性和可行性提供了科学依据。然而, 枸杞子作为一种多成分多功效的中药材, 仍需进一步探索造成不同等级枸杞子药效差异的关键物质基础; 同时应增加枸杞子的药效评价内容, 如明目作用、抗衰老作用等, 多角度多方面验证等级划分的科学性, 以满足实际生活中对枸杞子的不同需求。

本研究在充分兼顾枸杞子外观性状和内在品质之间的联系以及市场需求的基础上, 通过量化相关指标并规定划分范围, 将枸杞子划分为一等和统货两个等级。制定的标准从外观到内在、从主观到客观, 都更为准确合理地阐述了枸杞子的等级分类, 既符合传统的中药评价内容, 也具备一定的科学性和可行性, 对引导枸杞子市场优质优价的实现以及推动质量控制的提升具有重要意义。

作者贡献: 本文由余钟莲负责实验数据采集、文章撰写与修改; 李薛萍、刘文静参与数据处理; 杨莉、王峥涛、王瑞和石燕红负责样品收集、实验思路设计和稿件修改等工作。

利益冲突: 本文的作者和所涉及的内容不存在潜在的利益冲突。

基金

收起

上海市中医药三年行动计划(ZY(2021-2023)-0212)
上海市中医药三年行动计划(ZY(2021-2023)-0215)
公利医院国家自然科学基金培育计划项目(2023GPY-B04)

参考文献

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2024年第59卷第5期

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文章信息

doi: 10.16438/j.0513-4870.2023-1346

接收时间：2023-11-30
首发时间：2025-11-27
出版时间：2024-05-12

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出版历史

收稿日期：2023-11-30
修回日期：2024-02-17

基金

上海市中医药三年行动计划(ZY(2021-2023)-0212)

上海市中医药三年行动计划(ZY(2021-2023)-0215)

公利医院国家自然科学基金培育计划项目(2023GPY-B04)

作者信息

1.上海中医药大学中药学院, 上海 201203

2.上海中医药大学中医药国际标准化研究所, 上海 201203

3.上海市中医药国际标准化研究院, 上海 201203

4.上海中医药大学中药研究所, 中药标准化教育部重点实验室, 上海 201203

5.上海市浦东新区公利医院, 上海 200135

通讯作者:

^*王瑞, E-mail: ellewang@163.com;

石燕红, E-mail: shiyhtcm@shutcm.edu.cn

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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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No.	Habitat	Manufacturer	Batch	Grain number of 50 g	Length /mm	Diameter /mm	Imperfection /% (w/w)	Skin color^a
Goji-1	Ningxia Zhouta	Ningxia Zhouta	GQ-210623	281	15.76 ± 3.52	5.63 ± 0.89	3.01	1
Goji-2	GQ-210630	310	15.44 ± 2.90	5.78 ± 1.02	1.75	1
Goji-3	GQ-210709	321	15.31 ± 3.51	5.53 ± 1.16	0.94	1
Goji-4	GQ-210715	353	15.42 ± 3.69	6.10 ± 1.21	1.56	1
Goji-5	GQ-210723	330	15.26 ± 3.12	5.99 ± 1.29	1.90	1
Goji-6	GQ-210730	351	15.23 ± 1.79	5.82 ± 1.11	2.56	1
Goji-7	GQ-210623	283	16.40 ± 3.24	6.18 ± 1.24	3.02	1
Goji-8	GQ-210630	321	15.72 ± 2.44	5.62 ± 1.10	2.33	1
Goji-9	GQ-210709	331	15.31 ± 2.62	5.31 ± 1.13	2.81	1
Goji-10	Ningxia Xizan	Ningxia Xizan	GQ-210703	319	14.34 ± 2.42	5.75 ± 0.98	0.98	1
Goji-11	GQ-210710	332	15.43 ± 2.41	5.45 ± 1.15	1.52	1
Goji-12	GQ-210717	408	13.87 ± 0.95	5.46 ± 0.67	1.84	1
Goji-13	GQ-210724	410	13.05 ± 1.07	6.36 ± 0.94	1.92	1
Goji-14	GQ-210731	535	12.07 ± 1.52	5.48 ± 0.66	1.36	1
Goji-15	Ningxia Yinchuan	Ningxia Yinchuan	GQ-210706	558	11.52 ± 1.06	4.18 ± 0.70	3.57	1
Goji-16	GQ-210715	343	14.06 ± 1.85	5.32 ± 1.12	2.24	1
Goji-17	Ningxia Shizuishan	Ningxia Shizuishan	GQ-210617	331	15.55 ± 2.29	5.93 ± 1.17	0.88	1
Goji-18	GQ-210705	409	12.65 ± 0.77	4.81 ± 0.92	1.49	1
Goji-19	GQ-210615	271	15.34 ± 2.34	6.54 ± 1.20	2.67	1
Goji-20	GQ-210704	440	12.36 ± 1.68	4.38 ± 0.59	2.65	1
Goji-21	Ningxia	Shanghai Kangqiao	GQ-21090701	373	14.99 ± 1.80	5.83 ± 0.55	0.92	2
Goji-22	GQ-21090702	307	14.77 ± 2.33	5.75 ± 0.66	2.56	1
Goji-23	GQ-22081801	386	14.52 ± 2.52	5.49 ± 1.06	2.17	2
Goji-24	GQ-22081802	549	12.11 ± 1.82	4.61 ± 0.63	1.82	2
Goji-25	GQ-22081803	386	14.73 ± 2.14	5.81 ± 0.69	1.75	2
Goji-26	GQ-22081804	540	12.35 ± 1.27	4.74 ± 0.39	2.46	1
Goji-27	GQ-22081805	377	14.72 ± 2.63	6.19 ± 1.09	2.00	2
Goji-28	GQ-22081806	560	12.34 ± 2.32	4.71 ± 0.84	0.87	1
Goji-29	GQ-22081807	374	14.36 ± 2.32	5.98 ± 0.69	2.57	2
Goji-30	GQ-22081808	547	12.33 ± 1.70	4.75 ± 0.71	2.10	1
Goji-31	GQ-22081809	387	14.53 ± 3.12	5.96 ± 0.86	1.02	2
Goji-32	GQ-22081810	538	12.70 ± 1.28	4.20 ± 0.64	2.64	1

No.

Habitat

Manufacturer

Batch

Grain number of 50 g

Length /mm

Diameter /mm

Imperfection /% (w/w)

Skin color^a

Goji-1

Ningxia Zhouta

GQ-210623

281

15.76 ± 3.52

5.63 ± 0.89

3.01

Goji-2

GQ-210630

310

15.44 ± 2.90

5.78 ± 1.02

1.75

Goji-3

GQ-210709

321

15.31 ± 3.51

5.53 ± 1.16

0.94

Goji-4

GQ-210715

353

15.42 ± 3.69

6.10 ± 1.21

1.56

Goji-5

GQ-210723

330

15.26 ± 3.12

5.99 ± 1.29

1.90

Goji-6

GQ-210730

351

15.23 ± 1.79

5.82 ± 1.11

2.56

Goji-7

GQ-210623

283

16.40 ± 3.24

6.18 ± 1.24

3.02

Goji-8

GQ-210630

321

15.72 ± 2.44

5.62 ± 1.10

2.33

Goji-9

GQ-210709

331

15.31 ± 2.62

5.31 ± 1.13

2.81

Goji-10

Ningxia Xizan

GQ-210703

319

14.34 ± 2.42

5.75 ± 0.98

0.98

Goji-11

GQ-210710

332

15.43 ± 2.41

5.45 ± 1.15

1.52

Goji-12

GQ-210717

408

13.87 ± 0.95

5.46 ± 0.67

1.84

Goji-13

GQ-210724

410

13.05 ± 1.07

6.36 ± 0.94

1.92

Goji-14

GQ-210731

535

12.07 ± 1.52

5.48 ± 0.66

1.36

Goji-15

Ningxia Yinchuan

GQ-210706

558

11.52 ± 1.06

4.18 ± 0.70

3.57

Goji-16

GQ-210715

343

14.06 ± 1.85

5.32 ± 1.12

2.24

Goji-17

Ningxia Shizuishan

GQ-210617

331

15.55 ± 2.29

5.93 ± 1.17

0.88

Goji-18

GQ-210705

409

12.65 ± 0.77

4.81 ± 0.92

1.49

Goji-19

GQ-210615

271

15.34 ± 2.34

6.54 ± 1.20

2.67

Goji-20

GQ-210704

440

12.36 ± 1.68

4.38 ± 0.59

2.65

Goji-21

Ningxia

Shanghai Kangqiao

GQ-21090701

373

14.99 ± 1.80

5.83 ± 0.55

0.92

Goji-22

GQ-21090702

307

14.77 ± 2.33

5.75 ± 0.66

2.56

Goji-23

GQ-22081801

386

14.52 ± 2.52

5.49 ± 1.06

2.17

Goji-24

GQ-22081802

549

12.11 ± 1.82

4.61 ± 0.63

1.82

Goji-25

GQ-22081803

386

14.73 ± 2.14

5.81 ± 0.69

1.75

Goji-26

GQ-22081804

540

12.35 ± 1.27

4.74 ± 0.39

2.46

Goji-27

GQ-22081805

377

14.72 ± 2.63

6.19 ± 1.09

2.00

Goji-28

GQ-22081806

560

12.34 ± 2.32

4.71 ± 0.84

0.87

Goji-29

GQ-22081807

374

14.36 ± 2.32

5.98 ± 0.69

2.57

Goji-30

GQ-22081808

547

12.33 ± 1.70

4.75 ± 0.71

2.10

Goji-31

GQ-22081809

387

14.53 ± 3.12

5.96 ± 0.86

1.02

Goji-32

GQ-22081810

538

12.70 ± 1.28

4.20 ± 0.64

2.64

Item	Bright-red	Dark-red	Large size	Small size	First grade	Second grade
n	13	40	21	32	6	47
Length/mm	14.45 ± 2.29	14.60 ± 2.51	17.40 ± 0.92	12.70 ± 0.61	16.77 ± 0.38	14.28 ± 2.44
Diameter/mm	5.78 ± 0.54	5.56 ± 0.86	6.38 ± 0.45	5.11 ± 0.52	6.15 ± 0.43	5.55 ± 0.81
Moisture/%	7.37 ± 0.77^****	9.38 ± 1.07	8.96 ± 1.38	8.83 ± 1.30	7.26 ± 0.52^∆∆∆	9.09 ± 1.52
Ash/%	4.23 ± 0.19	4.24 ± 0.26	4.23 ± 0.25	4.24 ± 0.24	4.12 ± 0.12	4.25 ± 0.25
Water-soluble extractives/%	68.51 ± 3.17^*	64.67 ± 5.12	66.72 ± 4.88	64.88 ± 4.97	69.99 ± 3.70^∆	65.05 ± 4.86
Volatile ether extractives/%	0.62 ± 0.08	0.58 ± 0.09	0.58 ± 0.09	0.59 ± 0.09	0.64 ± 0.07	0.58 ± 0.09
LBP/%	3.02 ± 0.52^*	2.50 ± 0.65	2.68 ± 0.63	2.59 ± 0.68	2.98 ± 0.55	2.58 ± 0.66
Betaine/%	0.75 ± 0.16	0.85 ± 0.17	0.73 ± 0.13^##	0.88 ± 0.17	0.64 ± 0.11^∆∆	0.85 ± 0.16
AA-2βG/%	1.23 ± 0.14^****	0.72 ± 0.24	0.77 ± 0.33	0.89 ± 0.29	1.22 ± 0.18^∆∆	0.80 ± 0.29
ZD/%	0.27 ± 0.05^***	0.20 ± 0.06	0.23 ± 0.06	0.20 ± 0.07	0.28 ± 0.05^∆∆	0.20 ± 0.06

Item

Bright-red

Dark-red

Large size

Small size

First grade

Second grade

Length/mm

14.45 ± 2.29

14.60 ± 2.51

17.40 ± 0.92

12.70 ± 0.61

16.77 ± 0.38

14.28 ± 2.44

Diameter/mm

5.78 ± 0.54

5.56 ± 0.86

6.38 ± 0.45

5.11 ± 0.52

6.15 ± 0.43

5.55 ± 0.81

Moisture/%

7.37 ± 0.77^****

9.38 ± 1.07

8.96 ± 1.38

8.83 ± 1.30

7.26 ± 0.52^∆∆∆

9.09 ± 1.52

Ash/%

4.23 ± 0.19

4.24 ± 0.26

4.23 ± 0.25

4.24 ± 0.24

4.12 ± 0.12

4.25 ± 0.25

Water-soluble extractives/%

68.51 ± 3.17^*

64.67 ± 5.12

66.72 ± 4.88

64.88 ± 4.97

69.99 ± 3.70^∆

65.05 ± 4.86

Volatile ether extractives/%

0.62 ± 0.08

0.58 ± 0.09

0.59 ± 0.09

0.64 ± 0.07

0.58 ± 0.09

LBP/%

3.02 ± 0.52^*

2.50 ± 0.65

2.68 ± 0.63

2.59 ± 0.68

2.98 ± 0.55

2.58 ± 0.66

Betaine/%

0.75 ± 0.16

0.85 ± 0.17

0.73 ± 0.13^##

0.88 ± 0.17

0.64 ± 0.11^∆∆

0.85 ± 0.16

AA-2βG/%

1.23 ± 0.14^****

0.72 ± 0.24

0.77 ± 0.33

0.89 ± 0.29

1.22 ± 0.18^∆∆

0.80 ± 0.29

ZD/%

0.27 ± 0.05^***

0.20 ± 0.06

0.23 ± 0.06

0.20 ± 0.07

0.28 ± 0.05^∆∆

0.20 ± 0.06

Item	Length	Diameter	Skin color	Moisture	Ash	Water- soluble extractives	Volatile ether extractives	LBP	Betaine	AA-2βG	ZD
Length	1
Diameter	0.814^**	1
Skin color	-0.039	0.121	1
Moisture	0.078	-0.036	-0.669^**	1
Ash	-0.046	-0.154	-0.079	-0.090	1
Water-soluble extractives	0.199	0.179	0.343^*	-0.487^**	-0.099	1
Volatile ether extractives	-0.059	-0.108	0.225	-0.365^**	0.035	0.159	1
LBP	-0.067	-0.095	0.317^*	-0.104	0.038	0.006	0.124	1
Betaine	-0.371^**	-0.325^*	-0.236	0.125	0.013	-0.135	0.138	-0.005	1
AA-2βG	-0.305^*	-0.114	0.719^**	-0.414^**	-0.183	0.250	0.258	0.175	-0.033	1
ZD	0.083	0.074	0.496^**	-0.334^*	-0.053	0.159	-0.243	0.375^**	-0.384^**	0.469^**	1

Item

Length

Diameter

Skin color

Moisture

Ash

Water- soluble extractives

Volatile ether extractives

LBP

Betaine

AA-2βG

Length

Diameter

0.814^**

Skin color

-0.039

0.121

Moisture

0.078

-0.036

-0.669^**

Ash

-0.046

-0.154

-0.079

-0.090

Water-soluble extractives

0.199

0.179

0.343^*

-0.487^**

-0.099

Volatile ether extractives

-0.059

-0.108

0.225

-0.365^**

0.035

0.159

LBP

-0.067

-0.095

0.317^*

-0.104

0.038

0.006

0.124

Betaine

-0.371^**

-0.325^*

-0.236

0.125

0.013

-0.135

0.138

-0.005

AA-2βG

-0.305^*

-0.114

0.719^**

-0.414^**

-0.183

0.250

0.258

0.175

-0.033

0.083

0.074

0.496^**

-0.334^*

-0.053

0.159

-0.243

0.375^**

-0.384^**

0.469^**

Item	Grade
General information	Origin	Dried ripe fruit of Lycium barbarum L. (Fam. Solanaceae)
Wild/cultivated	Cultivated
Processing	Harvested in summer and fall when the fruit is red, dried in hot air, or aired until the skin is wrinkled, dried in the sun, then removing the pedicel
Morphological features	Shape	Nearly fusiform or elliptical
Surface feature	Stylar scars apically with small protuberant scars, basally with white fruiting pedicel scars
Texture	Pericarp is soft and externally roughly wrinkled; Sarcocarp is pulpy, soft and tender
Odor and taste	Slight; sweet
Seeds	20 to 50 seeds; brown-yellow; kidney-shaped and flat; 1.5-1.9 mm in length, 1-1.7 mm in diameter
Skin color	Bright-red	Dark-red
Grain number of 50 g	≤ 280	≤ 560
Length	≥ 16.00 mm	6.00-16.00 mm
Diameter	≥ 6.00 mm	3.00-6.00 mm
Imperfection	≤ 1.00%	≤ 3.00%
Test index	Moisture	≤ 8.00%	≤ 13.00%
Total ash	≤ 5.00%
Water-soluble extractives	≥ 70.00%	≥ 55.00%
Marker components contents	LBP	≥ 3.00%	≥ 1.80%
AA-2βG	≥ 1.00%	≥ 0.30%
ZD	≥ 0.25%	≥ 0.10%
Betaine	≥ 0.50%

Item

Grade

First

Second

General information

Origin

Dried ripe fruit of Lycium barbarum L. (Fam. Solanaceae)

Wild/cultivated

Cultivated

Processing

Harvested in summer and fall when the fruit is red, dried in hot air, or aired until the skin is wrinkled, dried in the sun, then removing the pedicel

Morphological features

Shape

Nearly fusiform or elliptical

Surface feature

Stylar scars apically with small protuberant scars, basally with white fruiting pedicel scars

Texture

Pericarp is soft and externally roughly wrinkled; Sarcocarp is pulpy, soft and tender

Odor and taste

Slight; sweet

Seeds

20 to 50 seeds; brown-yellow; kidney-shaped and flat; 1.5-1.9 mm in length, 1-1.7 mm in diameter

Skin color

Bright-red

Dark-red

Grain number of 50 g

≤ 280

≤ 560

Length

≥ 16.00 mm

6.00-16.00 mm

Diameter

≥ 6.00 mm

3.00-6.00 mm

Imperfection

≤ 1.00%

≤ 3.00%

Test index

Moisture

≤ 8.00%

≤ 13.00%

Total ash

≤ 5.00%

Water-soluble extractives

≥ 70.00%

≥ 55.00%

Marker components contents

LBP

≥ 3.00%

≥ 1.80%

AA-2βG

≥ 1.00%

≥ 0.30%

≥ 0.25%

≥ 0.10%

Betaine

≥ 0.50%