HPLC法测定不同产地栀子提取物的含量

doi:10.3969/j.issn.1001-1803.2022.04.016

摘要/Abstract

摘要：

通过高效液相色谱法（HPLC）测定不同产地栀子中主要成分栀子苷、栀子黄色素等含量,对不同产地的栀子进行比较。采用C₁₈（4.6 mm×250 mm,5 μm）色谱柱,水相为0.2%磷酸溶液,有机相为甲醇-乙腈,检测波长为254 nm,洗脱速度为1 mL/min,在柱温30 ℃条件下进行不同产地栀子中主要成分的测定。实验结果表明,供试品溶液的10种主要成分线性关系良好,平均加样回收率为97.3%~103.4%,通过比较不同产地栀子提取物含量的测定结果可知药材产地为江西平远县的栀子提取物中主要成分含量最高。

关键词: 栀子提取物, 高效液相色谱法, 有效成分, 机制研究

Abstract:

The contents of the main components of Gardenia, such as geniposide and gardenia yellow pigment, were determined by HPLC method, and the gardenia from different areas were compared. By using a C₁₈ （4.6 mm×250 mm, 5 μm） chromatographic column, the aqueous phase uses 0.2% phosphoric acid solution, the organic phase uses methanol-acetonitrile, the detection wavelength is 254 nm, the elution rate is 1 mL/min, and the column temperature is 30 ℃. The determination of the main components in Gardenia from different origins was carried out below. The experimental results show that the 10 main components of the solution have a good linear relationship, and the average sample recovery rate is 97.3%-103.4%. By comparing the determination results of Gardenia extracts from different origins, it can be seen that the Gardenia extract from Pingyuan County, Jiangxi Province has the highest amount of the main contents. The experimental method used in this paper has certain reliability and can help the medicinal research of Gardenia.

Key words: Gardenia extract, HPLC, active ingredient, mechanism study

中图分类号:

TQ658

武文涛,赵育林,刘亚智. HPLC法测定不同产地栀子提取物的含量[J]. 日用化学工业, 2022, 52(4): 451-456.

Wu Wentao,Zhao Yulin,Liu Yazhi. Determination of the content of Gardenia jasminoides Ellis from different producing areas by HPLC[J]. China Surfactant Detergent & Cosmetics, 2022, 52(4): 451-456.

图/表 4

表1

表2

加样回收试验结果（n=6）"

待测成分	取样量/g	样品含量/mg	加入量/mg	待测总量/mg	回收率/%	平均回收率/%	RSD/%
小檗碱	0.100 5	0.373 5	0.340 2	0.711 2	99.1	100.6	1.3
	0.100 7	0.374 2	0.340 2	0.710 8	101.7
	0.100 7	0.374 3	0.340 2	0.711 7	99.1
	0.100 3	0.372 8	0.340 2	0.713 6	100.1
	0.100 4	0.373 2	0.340 2	0.721 3	102.2
	0.100 3	0.372 8	0.340 2	0.716 2	100.8
黄岑苷	0.100 5	0.620 9	0.580 8	1.211 1	101.5	103.3	1.0
	0.100 7	0.621 2	0.580 8	1.223 7	103.4
	0.100 7	0.621 2	0.580 8	1.218 3	102.5
	0.100 3	0.618 7	0.580 8	1.220 5	103.3
	0.100 4	0.620 3	0.580 8	1.228 3	104.6
	0.100 5	0.620 9	0.580 8	1.223 6	103.7
汉黄岑苷	0.100 5	0.241 4	0.227 9	0.464 0	98.0	99.9	1.3
	0.100 7	0.241 9	0.227 9	0.479 4	100.0
	0.100 7	0.241 9	0.227 9	0.465 7	98.5
	0.100 3	0.240 9	0.227 9	0.468 2	100.0
	0.100 4	0.240 2	0.227 9	0.472 2	101.7
	0.100 3	0.240 9	0.227 9	0.479 2	100.4
黄岑素	0.010 13	0.171 7	0.135 8	0.313 7	103.5	102.7	1.4
	0.010 06	0.170 5	0.135 8	0.308 7	100.8
	0.010 18	0.174 3	0.135 8	0.313 2	101.3
	0.010 10	0.171 2	0.135 8	0.315 9	104.8
	0.010 17	0.172 4	0.135 8	0.312 8	102.5
	0.010 03	0.170 2	0.135 8	0.311 1	103.0
栀子黄色素	0.100 5	0.030 3	0.025 4	0.056 3	102.6	103.3	0.7
	0.100 7	0.030 2	0.025 4	0.056 6	103.5
	0.100 7	0.030 2	0.025 4	0.056 3	102.4
	0.100 3	0.030 1	0.025 4	0.056 3	103.0
	0.100 4	0.030 1	0.025 4	0.056 7	104.3
	0.100 3	0.030 1	0.025 4	0.056 5	103.6
汉黄岑素	0.100 5	0.491 3	0.491 9	1.000	103.3	103.4	0.8
	0.100 7	0.491 5	0.491 9	1.000	103.1
	0.100 7	0.491 3	0.491 9	0.995 9	102.3
	0.100 3	0.490 3	0.491 9	0.994 9	102.5
	0.100 4	0.490 8	0.491 9	1.005	104.6
	0.100 3	0.499 3	0.491 9	1.000	103.8
大黄酸	0.101 4	0.072 2	0.057 9	0.139 6	100.5	102.1	1.5
	0.101 8	0.072 5	0.057 9	0.139 6	100.0
	0.101 0	0.071 9	0.057 9	0.131 0	103.6
	0.101 6	0.071 3	0.057 9	0.131 4	103.5
	0.101 6	0.071 3	0.057 9	0.131 1	103.0
	0.101 4	0.071 2	0.057 9	0.130 1	101.5
大黄素	0.101 4	0.061 4	0.069 9	0.131 2	99.6	99.2	0.5
	0.101 9	0.061 7	0.069 9	0.130 6	98.4
	0.101 0	0.061 1	0.069 9	0.131 9	99.6
	0.101 6	0.061 5	0.069 9	0.130 7	98.7
	0.101 6	0.061 5	0.069 9	0.131 0	99.2
	0.101 4	0.061 4	0.069 9	0.131 0	99.2
大黄酚	0.101 4	0.128 3	0.119 8	0.241 8	96.9	97.3	0.7
	0.101 8	0.129 9	0.119 8	0.242 0	96.5
	0.101 0	0.127 8	0.119 8	0.243 0	97.4
	0.101 6	0.128 6	0.117 0	0.243 7	97.3
	0.101 6	0.128 6	0.117 0	0.242 8	96.8
	0.101 4	0.128 3	0.117 0	0.243 1	97.1
栀子苷	0.101 4	0.036 9	0.026 9	0.063 7	99.0	100.3	1.5
	0.101 9	0.037 1	0.026 9	0.063 7	99.8
	0.101 0	0.036 8	0.026 9	0.063 9	100.4
	0.101 6	0.037 0	0.026 9	0.064 0	101.8
	0.101 6	0.037 0	0.026 9	0.063 8	99.8
	0.101 4	0.036 0	0.026 9	0.064 6	101.2

表2

表3

表4

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成分	回归方程	相关系数r	线性范围/（μg/mL）
盐酸小檗碱	Y=4.45×10⁶X-3.28×10⁴	0.999	0.053 5~1.25
黄岑苷	Y=3.32×10⁶X+1.05×10⁴	1.000	0.052 8~1.77
汉黄岑苷	Y=3.67×10⁶X-1.73×10⁴	0.999	0.053 0~1.83
黄岑素	Y=5.31×10⁶X-9.47×10⁴	0.999	0.207 0~7.53
栀子黄色素	Y=4.53×10⁶X-3.09×10³	0.999	0.005 56~0.187
汉黄岑素	Y=5.78×10⁶X-4.23×10⁴	0.999	0.071 8~2.43
大黄酸	Y=4.94×10⁶X-6.18×10³	0.999	0.005 18~0.745
大黄素	Y=3.35×10⁶X-4.91×10³	0.999	0.006 28~0.212
大黄酚	Y=5.08×10⁶X-9.92×10³	0.999	0.017 0~0.598
栀子苷	Y=3.35×10⁶X-2.57×10³	0.999	0.005 08~0.179

序号	保留时间/min
	大黄素	小檗碱		黄岑苷		汉黄岑苷		黄岑素		栀子黄色素		汉黄岑素		大黄酸		大黄酚		栀子苷
	ESM	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS
1	64.68	13.83	14.31	21.86	22.20	29.85	30.24	37.04	37.01	45.12	45.08	47.15	47.01	51.24	51.61	74.84	75.10	80.58	81.11
2	64.67	13.77	14.32	21.82	22.21	29.83	30.25	37.05	37.02	45.13	45.07	47.13	47.04	51.26	51.62	74.83	75.11	80.56	81.04
3	64.51	13.79	14.16	21.74	22.15	29.79	30.19	36.85	36.76	45.00	44.83	47.09	46.78	51.18	51.46	74.68	74.85	80.54	80.74
4	64.53	13.73	14.16	21.78	22.15	29.84	30.18	36.87	36.76	45.02	44.87	47.11	46.78	51.14	51.46	74.66	74.93	80.55	80.73
5	64.58	13.74	14.13	21.74	22.12	29.72	30.16	36.89	36.73	45.03	44.89	47.04	46.75	51.15	51.42	74.67	74.92	80.53	80.71
6	64.54	13.72	14.16	21.77	22.16	29.83	30.19	36.85	36.76	45.06	44.91	47.15	46.78	51.19	51.46	74.68	74.97	80.56	80.74
7	64.53	13.83	14.29	21.76	22.28	29.73	30.23	36.82	36.95	45.07	45.02	47.12	47.01	51.16	51.68	74.82	75.08	80.57	80.87
8	64.69	13.78	14.24	21.79	22.23	29.75	30.26	36.85	36.85	45.05	45.01	47.14	46.82	51.15	51.58	74.69	75.03	80.52	80.82
9	64.68	13.89	14.25	21.77	22.25	29.84	30.27	36.94	36.84	45.13	45.04	47.16	46.86	51.14	51.54	74.77	75.02	80.58	80.84
10	64.63	13.75	14.27	21.75	22.21	29.81	30.24	36.85	36.82	45.08	45.00	47.12	46.84	51.13	51.52	74.75	75.01	80.59	80.80

序号	含量/（mg/g）
	大黄素	小檗碱		黄岑苷		汉黄岑苷		黄岑素		栀子黄色素		汉黄岑素		大黄酸		大黄酚		栀子苷
	ESM	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS	ESM	QAMS
1	0.243	3.35	3.28	1.14	1.05	0.654	0.672	3.79	3.00	0.138	0.135	5.38	5.28	0.271	0.263	0.603	0.601	0.157	0.145
2	0.531	1.79	1.67	8.36	8.46	2.08	2.08	4.08	4.01	0.287	0.272	1.71	1.82	0.535	0.526	1.06	1.65	0.401	0.329
3	0.192	3.51	3.48	18.79	18.17	4.01	4.05	3.59	3.37	0.143	0.149	2.13	2.02	0.263	0.253	1.53	0.526	0.118	0.106
4	0.220	1.73	1.78	13.49	13.58	3.28	3.28	5.03	4.76	0.157	0.152	1.82	1.75	0.205	0.205	0.538	0.664	0.173	0.169
5	0.170	3.64	3.57	1.73	1.76	0.41	0.525	2.15	2.07	0.112	0.12	0.72	0.79	0.029	0.026	0.667	1.05	0.374	0.374
6	0.192	2.58	2.58	3.85	4.00	3.07	3.15	6.29	5.69	0.086	0.083	3.33	3.26	0.200	0.201	0.42	0.417	0.089	0.098
7	0.416	3.79	3.69	21.79	22.00	13.68	6.86	9.40	9.25	0.158	0.145	6.61	6.53	0.486	0.498	1.503	1.507	0.625	0.626
8	0.151	2.81	2.76	1.72	1.75	1.13	1.17	7.58	7.07	0.127	0.124	3.58	3.46	0.219	0.281	0.252	0.258	0.052	0.052
9	0.225	1.10	1.07	4.51	4.56	6.82	1.04	3.48	3.36	0.103	0.109	1.27	1.33	0.152	0.163	1.08	1.08	0.308	0.302
10	0.213	3.43	3.35	23.39	24.78	6.79	6.12	2.04	2.06	0.135	0.139	1.15	1.29	0.565	0.578	0.274	0.272	0.115	0.109

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