HPLC-MS/MS法同时测定脑复清胶囊中11种成分  

Simultaneous determination of 11 components in Naofuqing Capsule by HPLC-MS/MS

作　　者：陈红英 张容华 CHEN Hong-ying;ZHANG Rong-hua(Baiyunshan Pharmaceutical General Factory,Guangzhou Baiyunshan Pharmaceutical Group Co.,Ltd.,Guangzhou 510515,China)

机构地区：[1]广州白云山医药集团股份有限公司白云山制药总厂,广东广州510515

出　　处：《中草药》2018年第15期3645-3650,共6页Chinese Traditional and Herbal Drugs

摘　　要：目的建立一种高效液相色谱串联质谱(HPLC-MS/MS)分析方法,可同时测定脑复清胶囊中刺五加苷E、2,3,5,4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(二苯乙烯苷)、异嗪皮啶、迷迭香酸、三七皂苷R1、丹酚酸B、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd和大黄素共11种成分的含量。方法采用Agilent Poroshell 120 EC-C18(75 mm×4.6 mm,2.7μm)色谱柱,以0.1%甲酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱,体积流量0.4 m L/min,柱温35℃。质谱采用负离子多反应监测模式进行检测。结果 11个成分在各自浓度范围内线性关系良好(r>0.996),刺五加苷E、二苯乙烯苷、异嗪皮啶、迷迭香酸、三七皂苷R1、丹酚酸B、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd、大黄素的加样回收率分别为106.4%、104.2%、99.9%、102.3%、104.1%、98.3%、108.9%、103.6%、105.8%、101.9%、104.2%;11种成分在10批样品中的质量分数分别为0.274~0.310 mg/g、1.579~1.642 mg/g、0.093~0.099 mg/g、0.331~0.352 mg/g、1.115~1.229 mg/g、1.663~1.870 mg/g、4.884~5.173 mg/g、0.691~0.762 mg/g、2.974~3.358 mg/g、1.053~1.493 mg/g、0.100~0.115 mg/g。结论所建立的方法灵敏度高,稳定快速,适用于同时测定脑复清胶囊中11个成分的含量,可以用于该产品质量控制。Objective To develop a high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method for simultaneous determination of 11 components including eleutheroside E, 2,3,5,4′-tetera-hydroxystilbene-2-O-β-D-glucoside（stilbene glycoside）, isofraxidin, rosmarinic acid, notoginsenoside R1, salvianolic acid B, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd, and emodin in Naofuqing Capsule. Methods The analysis was performed on an Agilent Poroshell 120 EC-C18 column（75 mm × 4.6 mm, 2.7 μm）, and the mobile phase consisted of water containing 0.1% formic acid and acetonitrile with gradient elution at the flow rate of 0.4 m L/min. The column temperature was maintained at 35 ℃. The MS detection for the 11 tested components was performed in negative ion multiple reaction monitoring mode. Results Good linear relationship were observed in the test range for 11 components, and the recoveries of eleutheroside E, stilbene glycoside, isofraxidin, rosmarinic acid, notoginsenoside R1, salvianolic acid B, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd, and emodin were 106.4%, 104.2%, 99.9%, 102.3%, 104.1%, 98.3%, 108.9%, 103.6%, 105.8%, 101.9%, and 104.2%, respectively. The contents of 10 batches of the 11 components were in the ranges of 0.274—0.310, 1.579—1.642, 0.093—0.099, 0.331—0.352, 1.115—1.229, 1.663—1.870, 4.884—5.173, 0.691—0.762, 2.974—3.358, 1.053—1.493, and 0.100—0.115 mg/g, respectively. Conclusion The established method is sensitive, stable, and rapid. It is suitable for the simultaneous determination of multiple components in Naofuqing Capsule.

关 键 词：脑复清胶囊 HPLC-MS/MS 刺五加苷E 二苯乙烯苷 异嗪皮啶 迷迭香酸 三七皂苷R1 丹酚酸B 人参皂苷Rg1 人参皂苷RE 人参皂苷Rb1 人参皂苷RD 大黄素 

分 类 号：R286.02[医药卫生—中药学]