市售保健品中7种醒酒护肝功效成分的毛细管电泳测定

doi:10.7503/cjcu20150980

摘要/Abstract

摘要：

采用胶束电动毛细管电泳-二极管阵列检测器同时检测了市售保健品中儿茶素、表儿茶素、表没食子儿茶素、表儿茶素没食子酸酯、表没食子儿茶素没食子酸酯、二氢杨梅素和甘草酸等7种醒酒护肝功效成分. 采用正交设计法对毛细管电泳条件[缓冲剂浓度、添加剂十二烷基硫酸钠(SDS)浓度、添加剂乙腈比例以及电泳缓冲溶液pH]进行了优化. 在优化的条件下, 7种组分在各自的线性范围内相关系数r≥0.9989, 检出限和定量限分别为0.26~2.22 μg/g(S/N=3)和0.87~7.39 μg/g(S/N=10), 日内精密度和日间精密度分别为1.3%~2.5%和1.9%~3.9%, 样品加标回收率为91.4%~104.9%, 加标样品的相对标准偏差(RSD)在1.4%~3.2%之间. 本方法可在8 min内实现7种功效成分的同时检测, 能够满足市售醒酒护肝产品的常规分析和质量评价要求.

关键词: 胶束电动毛细管电泳, 正交设计, 儿茶素, 二氢杨梅素, 甘草酸

Abstract:

A rapid method of micellar electrokinetic capillary electrophoresis(CE) coupled with diode array detection was developed for simultaneous determination of catechin, epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, dihydromyricetin and glycyrrhizic acid in functional food for anti-hangover and hepatoprotection. The parameters of capillary electrophoresis, including buffer concentration, concentration of sodium dodecyl sulfate(SDS), volume ratio of acetonitrile, and pH of the buffer, were optimized with orthogonal design. Under the optimal analytical conditions, the peak area of each analyte and its concentration had a good correlation within the linear range(r≥0.9989). Limit of detection(LOD) and quantification(LOQ) of the method were in the range of 0.26—2.22 μg/g(S/N=3) and 0.87—7.39 μg/g(S/N=10), respectively. The intra- and inter-day relative standard deviations(RSDs) of the mixed standard solution were 1.3%—2.5% and 1.9%—3.9%, respectively. While the spiked recoveries of the analytes were 91.4%—104.9% and the RSDs of the spiked samples were 1.4%—3.2%. The method of capillary electrophoresis for determination of the 7 components in functional food for anti-hangover and hepatoprotection was proposed in this study and could achieve baseline separation for all the target components within 8 min. The results show that the method could meet the requirement for routine analysis and quality control and evaluation.

Key words: Micellar electrokinetic capillary electrophoresis, Orthogonal design, Catechin, Dihydromyricetin, Glycyrrhizic acid(Ed.: D, K)

中图分类号:

O657.8

TrendMD:

邹海民, 周琛, 孙成均, 李永新, 杨晓松, 文君, 曾红燕. 市售保健品中7种醒酒护肝功效成分的毛细管电泳测定. 高等学校化学学报, 2016, 37(7): 1276.

ZOU Haimin, ZHOU Chen, SUN Chengjun, LI Yongxin, YANG Xiaosong, WEN Jun, ZENG Hongyan. Simultaneous Determination of 7 Components in Functional Food for Anti-hangover and Hepatoprotection by Capillary Electrophoresis^†. Chem. J. Chinese Universities, 2016, 37(7): 1276.

图/表 6

参考文献 21

[1]	Svoboda P., VlćckováH. , NovákováL. , J. Pharm. Biomed. Anal. , 2015, 114, 62—70
[2]	Ye L. Y., Wang H. J., Duncan S. E., Eigel W. N., O’Keefe S. F., Food Chem., 2015, 172, 416—422
[3]	Charpe T. W., Rathod V. K., Food Bioprod. Process,2015, 93, 51—57
[4]	Shabkhiz M. A., Eikani M. H., Bashiri Sadr Z., Golmohammad F., Food Chem., 2016, 210, 396—401
[5]	Liu G. Q., Dong J., Wang H., Wan L. R., Duan Y.S., Chen S. Z., Chem. J. Chinese Universities,2009, 30(8), 1566—1570(刘国强, 董静, 王弘, 万乐人, 端裕树, 陈世忠. 高等学校化学学报, 2009, 30(8), 1566—1570)
[6]	Anissi J., El Hassouni M., Ouardaoui A., Sendide K., Food Chem., 2014, 150, 438—447
[7]	Oh J., Jo H., Cho A. R., Kim S. J., Hanet J., Food Control,2013, 31(2), 403—409
[8]	Ou X. H., Ye Y., Huang Q. J., Liu H. G., Song Y. F., Nat. Prod. Res. Dev., 2013, 25(2), 245—248(欧贤红, 叶勇, 黄秋洁, 刘华钢, 宋云飞. 天然产物研究与开发, 2013, 25(2), 245—248)
[9]	Fu Y., Chen J., Li Y. J., Zheng Y. F., Li P., Food Chem., 2013, 141(2), 1063—1071
[10]	Wang X.Y., Zhang H, Chen L. L., Shan L. H., Fan G. W., Gao X. M., J. Ethnopharmacol., 2013, 150(3), 781—790
[11]	Boudesocque L., Dorat J., Pothier J., Gueiffer A., Gueiffier C. E., Food Chem., 2013, 139, 866—871
[12]	Soleas G. J., Yan J., Goldberg D. M., J. Chromatogr. B,2001, 757(1), 161—172
[13]	Liao W. C., Lin Y. H., Chang T. M., Huang W. Y., Food Chem., 2012, 132(4), 2188—2193
[14]	Rahim A. A., Nofrizal S., Saad B., Food Chem., 2014, 147, 262—268
[15]	Peres R. G., Tonin F. G., Tavares M. F. M., Amaya D. B. R., Food Chem., 2011, 127(2), 651—655
[16]	Zhang S., Dong S. Q., Chi L. Z., He P. G., Wang Q. J., Fang Y. Z., Talanta,2008, 76(4), 780—784
[17]	Vinatoru M., Ultrason. Sonochem., 2001, 8(3), 303—313
[18]	Morelli L. L. L., Prado M. A., Ultrason. Sonochem., 2012, 19(6), 1144—1149
[19]	Lun S. Y., Leung L. K., Huang Y., Chen Z. Y., Food Chem., 2003, 83(2), 189—195
[20]	Ananingsih V. K., Sharma A., Zhou W. B., Food Res. Int., 2013, 50(2), 469—479
[21]	Xu J. J., Yao M. J., Wu M. C., Food Sci., 2008, 29(11), 622—625(徐静娟, 姚茂君, 邬敏辰. 食品科学, 2008, 29(11), 622—625)

Compound	Regression equation	Correlation coefficient	Linear range/(μg·mL^-1)	LOD/(μg·g^-1)	LOQ/(μg·g^-1)
EGC	y=3049.1x-13.5	0.9995	0.09—100	0.55	1.83
C	y=4294.2x+17.9	0.9994	0.06—100	0.34	1.13
EC	y=4892.8x+27.4	0.9991	0.05—100	0.26	0.87
EGCG	y=3343.5x-33.1	0.9993	0.12—100	0.79	2.64
ECG	y=5521.2x+22.7	0.9989	0.08—100	0.63	2.09
DMY	y=3940.3x-15.5	0.9993	0.16—100	1.00	3.32
GA	y=897.2x+11.9	0.9992	0.35—200	2.22	7.39

Compound	Regression equation	Correlation coefficient	Linear range/(μg·mL^-1)	LOD/(μg·g^-1)	LOQ/(μg·g^-1)
EGC	y=3049.1x-13.5	0.9995	0.09—100	0.55	1.83
C	y=4294.2x+17.9	0.9994	0.06—100	0.34	1.13
EC	y=4892.8x+27.4	0.9991	0.05—100	0.26	0.87
EGCG	y=3343.5x-33.1	0.9993	0.12—100	0.79	2.64
ECG	y=5521.2x+22.7	0.9989	0.08—100	0.63	2.09
DMY	y=3940.3x-15.5	0.9993	0.16—100	1.00	3.32
GA	y=897.2x+11.9	0.9992	0.35—200	2.22	7.39

Compound	Intra-day precision(RSD, %)		Inter-day precision(RSD, %)
Compound	Retention time	Area	Retention time	Area
EGC	0.41	1.3	0.92	1.9
C	0.32	1.5	1.0	2.3
EC	0.54	1.9	1.3	2.8
EGCG	0.52	2.5	1.5	3.7
ECG	0.61	2.1	1.7	3.9
DMY	0.68	2.3	1.2	3.2
GA	0.77	1.7	1.4	2.6

Compound	Intra-day precision(RSD, %)		Inter-day precision(RSD, %)
Compound	Retention time	Area	Retention time	Area
EGC	0.41	1.3	0.92	1.9
C	0.32	1.5	1.0	2.3
EC	0.54	1.9	1.3	2.8
EGCG	0.52	2.5	1.5	3.7
ECG	0.61	2.1	1.7	3.9
DMY	0.68	2.3	1.2	3.2
GA	0.77	1.7	1.4	2.6

Compound	Background/(μg·mL^-1)	Added/(μg·mL^-1)	Found/(μg·mL^-1)	Recovery(%)	RSD(%)
EGC	8.27	5.00	13.0	93.9	2.7
		10.00	17.9	95.7	2.3
		20.00	27.4	95.4	2.9
C	ND	5.00	4.66	93.1	3.2
		10.00	9.48	94.8	2.7
		20.00	19.3	96.5	2.6
EC	5.88	5.00	10.4	94.1	2.5
		10.00	15.4	97.8	2.7
		20.00	26.1	102.1	1.8
EGCG	27.23	10.00	37.0	96.4	2.2
		20.00	46.6	96.2	1.4
		40.00	69.4	104.9	1.7
ECG	10.30	5.00	14.8	93.4	3.1
		10.00	19.2	91.4	2.8
		20.00	29.6	97.5	3.0
DMY	ND	5.00	4.60	92.1	3.2
		10.00	9.35	93.5	2.6
		20.00	18.3	91.6	2.2
GA	ND	20.00	20.7	103.3	2.3
		40.00	39.2	98.1	1.8
		80.00	81.8	102.2	1.7