心可宁胶囊中违法染色成分酸性红73检测方法的研究  

Research on the detection methods of illegal dyeing ingredient acid red 73 in the Xinkening capsules

作　　者：胡亮 罗时 李瑞莲 罗疆南 HU Liang;LUO Shi;LI Rui-lian;LUO Jiang-nan(Hunan Institute for Drug Control,Hunan Pharmaceutical Excipients Testing and Inspection Center,Changsha 410001,China;Hunan Engineering&Technology Research Center for Phannaceutical Quality Evaluation,Changsha 410001,China)

机构地区：[1]湖南省药品检验研究院湖南药用辅料检验检测中心,长沙410001 [2]湖南省药品质量评价工程技术研究中心,长沙410001

出　　处：《药物分析杂志》2019年第8期1489-1494,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:确认心可宁胶囊中违法染色的色素或染料成分,建立相应的染色成分分析方法。方法:采用高效液相色谱(HPLC)法对心可宁胶囊进行筛查,并采用HPLC-MS/MS二级质谱对阳性样品进行确认。质谱采用电喷雾负离子扫描(ESI-),多反应监测模式(MRM),选择质荷比m/z 255.0→150.5和m/z255.0→241.0作为检测离子对,记录相应色谱图。在此基础上,采用HPLC法对阳性样品中的酸性红73进行含量测定。色谱条件:采用Hypersil ODS色谱柱(250 mm×4.6 mm,5μm)),以乙腈-0.05 mol·L^-1醋酸铵溶液(24∶76)为流动相,流速为0.8 mL·min^-1,检测波长为509 nm。结果:采用HPLC法对213批心可宁胶囊进行筛查,并采用HPLC-MS/MS对可疑样品进行确认,有24批样品可检出酸性红73;酸性红73进样量在0.001 203~1.203μg的范围内乌峰面积有良好的线性关系。24批阳性样品中酸性红73的含量范围为6.25~87.6μg·g^-1。结论:本方法准确可靠,可作为心可宁胶囊中酸性红73染色物的检测方法。Objective:The purpose of the research is to establish an analysis method for identification of the pigments or dyes in Xin Kening capsules.Methods:An HPLC was used as the screening method of acid red 73.The positive results of screening were confirmed by HPLC-MS/MS with ESI-ion source.The ion at m/z 255.0 → 150.5 and m/z 255.0 → 241.0 was selected for MS/MS analysis and the corresponding chromatogram was recorded. Based on those results,an HPLC method was developed for the qualification of acid red 73 in positive samples.An Hypersil ODS C18(250 mm×4. 6 mm,5 μm)column was adopted,the mixture of acetonitrile and 0.05 mol·L^-1 a mmonium acetate(24∶76)was used as the mobile phase,the flow rate was 0.8 mL·min^-1,and the detection wavelength was set at 509 nm.Results:The HPLC method was used for the screening of 213 batches of Xin Kening capsules.The suspected samples were confirmed by HPLC-MS/MS.Acid red 73 was detected from 213 batches of samples.Acid red 73 had considerable linear relationship in the range of 0.001 203-1.203 μg.The content of acid red 73 in 24 batches of positive samples ranged from 6.25 to 87.6 μg·g^-1. Conclusion:This method is accurate and reliable,and can be used as the detection method for acid red 73 in Xin Kening capsules.

关 键 词：心可宁胶囊 酸性红73 化工染料 高效液相色谱法 液相色谱-质谱联用法 安全监测 

分 类 号：R917[医药卫生—药物分析学]