盐酸兰地洛尔原料药中3-［4-(3-硝基苯磺酰氧基)苯基］丙酸的检测方法学研究

doi:10.3976/j.issn.1002-4026.2017.02.017

山东科学 ›› 2017, Vol. 30 ›› Issue (2): 113-120.doi: 10.3976/j.issn.1002-4026.2017.02.017

盐酸兰地洛尔原料药中3-［4-(3-硝基苯磺酰氧基)苯基］丙酸的检测方法学研究

王珊珊¹，王丽娟¹，李卓瓦²，宁凡盛¹，王晓利¹，陈跃¹，陈相峰^1*

1.山东省分析测试中心，山东济南250014；2.枣庄学院，山东枣庄277000

收稿日期:2017-01-18
通信作者: 陈相峰（1981—），男，博士，副研究员，研究方向为质谱分析。E-mail：xiangfchensdas@163.com E-mail:xiangfchensdas@163.com
作者简介:王珊珊（1983—），女，博士，研究方向为分析化学。
基金资助:
山东省自然科学基金（ZR2012BQ009）

Study on detecting method of 3-［4-(3-nitrobenzene sulfonyl oxygen radicals) phenyl］ propionic acid in the landiolol hydrochloride crude drug

WANG Shan-shan¹,WANG Li-juan¹, LI Zhuo-wa², NING Fan-sheng¹,WANG Xiao-li¹, CHEN Yue¹, CHEN Xiang-feng^1*

1. Shandong Analysis and Test Center, Jinan 250014, China; 2.Zaozhuang College,Zaozhuang 277000, China

Received:2017-01-18

摘要/Abstract

摘要：

为了检测并控制合成盐酸兰地洛尔原料药物的质量，依托高效液相色谱-三重串联四级杆质谱建立了一种测定其中痕量基因毒性杂质3-［4-(3-硝基苯磺酰氧基)苯基］丙酸的方法。方法采用多级反应监测模式，检测灵敏度可达到0.50 mg/kg，加标回收率在91.9% ~ 97.8%之间，且精密度的相对标准偏差为3.28%(n=6)，均能满足杂质检测的需要。该研究方法操作简单、结果可靠，可实现快速、低成本检测。

关键词: 液相色谱-三重串联四级杆质谱, 3-［4-(3-硝基苯磺酰氧基)苯基］丙酸, 痕量检测, 盐酸兰地洛尔

Abstract:

To detect and control the content of trace toxic impurity 3-［4-(3-nitrobenzene sulfonyl oxygen radicals) phenyl］ propionic acid, which isessential material in the synthesis of landiolol hydrochloride drug, a HPLC with tandem mass spectrometry method was developed to determine the 3-［4-(3-nitrobenzene sulfonyl oxygen radicals) phenyl］ propionic acid in the landiolol hydrochloride crude drug. The multiple reaction monitor mode was used to eliminate the matrix effect and increase the sensitivity of the method. The limit of detection of the target analyte was 0.50 mg/kg. The recoveries of spiked samples were between 91.9% and 97.8%. The relative standard diviation value of precision experiment was 3.28%(n=6). The established method was simple, reliable, fast and low cost,which is able to meet the demand of impurities determination in crude drugs.

Key words: landiolol hydrochloride, 3-［4-(3-nitrobenzene sulfonyl oxygen radicals)phenyl］propionic acid;trace detection, high performance liquid chromatography with tandem mass spectrometry

中图分类号:

O656.31

王珊珊，王丽娟，李卓瓦，宁凡盛，王晓利，陈跃，陈相峰. 盐酸兰地洛尔原料药中3-［4-(3-硝基苯磺酰氧基)苯基］丙酸的检测方法学研究[J]. 山东科学, 2017, 30(2): 113-120.

WANG Shan-shan,WANG Li-juan, LI Zhuo-wa, NING Fan-sheng,WANG Xiao-li, CHEN Yue, CHEN Xiang-feng. Study on detecting method of 3-［4-(3-nitrobenzene sulfonyl oxygen radicals) phenyl］ propionic acid in the landiolol hydrochloride crude drug[J]. SHANDONG SCIENCE, 2017, 30(2): 113-120.

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