UHPLC-MS Determination of 7 Lignans in Schisandra Vinegar Products
摘 要
采用超高效液相色谱-质谱法测定醋五味子中五味子酯甲、五味子酚、五味子甲素、五味子乙素、五味子丙素、五味子醇甲和五味子醇乙等7种木脂素的含量。醋五味子样品0.200 0 g用甲醇10 mL超声提取30 min。以ACQUITY UPLC BEH C18色谱柱为分离柱,以不同体积比的乙腈和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱,质谱分析中采用电喷雾正离子源和选择离子监测模式。7种木脂素的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.001~0.050 mg·L-1。对6.0 mg·L-1的7种木脂素混合标准溶液连续测定6次,测定值的相对标准偏差为1.2%~3.5%。方法用于醋五味子样品的分析,加标回收率为85.4%~99.3%。
Abstract
UHPLC-MS was applied to the determination of 7 lignans, i.e. Schisantherrin A, Schisanhenol, Deoxyschisandrin, Schisandrin B, Schisandrin C, Schisandrin and Schisandrol B in Schisandra vinegar products. The sample (0.200 0 g) was extracted ultrasonically with methanol (10 mL) for 30 min. ACQUITY UPLC BEH C18 chromatographic column was used as stationary phase, and the mixture of acetonitrile and 0.1% (φ) formic acid solution mixed in different ratios was used as mobile phase in gradient elution. ESI+ and the selected ion monitoring mode were adopted in MS. Linear relationships between values of peak area and mass concentration of the 7 lignans were kept in definite ranges. Detection limits (3S/N) of the method ranged from 0.001 to 0.050 mg·L-1. Precision of the method was tested at the concentration level of 6.0 mg·L-1 of the 7 lignans mixed standard solution for 6 determinations, values of RSDs found were in the range of 1.2%-3.5%. The proposed method was applied to the analysis of samples of Schisandra vinegar products, giving values of recovery in the range of 85.4%-99.3%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201808006
所属栏目 工作简报
基金项目 国家自然科学基金(81403067);省自然科学基金(C2016059)
收稿日期 2017/8/31
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备注王哲,实验师,硕士,主要从事质谱分析工作,zhew0316@163.com
引用该论文: WANG Zhe,SHEN Shuchang,XIN Yang. UHPLC-MS Determination of 7 Lignans in Schisandra Vinegar Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(8): 896~900
王哲,申书昌,辛杨. 超高效液相色谱-质谱法测定醋五味子中7种木脂素的含量[J]. 理化检验-化学分册, 2018, 54(8): 896~900
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【3】高慧,佟鑫,裴启洋,等.五味子醋制过程中6种木脂素成分含量变化[J].中国实验方剂学杂志, 2014,20(19):32-34.
【4】窦志华,安莉萍,陈敏,等.一测多评法同时测定五味子中6种木脂素类成分含量[J].中国药学杂志, 2014,49(2):147-151.
【5】汪丽君,刘淑敏,毛春芹,等.一测多评法同时测定五味子中8种木质素类成分含量[J].药物分析杂志, 2015,35(7):1191-1197.
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【7】黄致君,陈衡霞,陆兔林,等.HPLC法测定不同产地醋五味子中6种木脂素类成分的含量[J].南京中医药大学学报, 2012,28(3):272-274.
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