金胺O染色物在中成药中的检测方法研究  

Study on detection methods for auramine O in Chinese patent medicines

作　　者：余新启[1,2] 何轶[2] 鲁静[2] 何风艳[2] 戴忠[2] 林瑞超[2] 马双成[2] 

机构地区：[1]黄石市食品药品检验所,黄石435000 [2]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2014年第1期130-135,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：公益性行业科研专项资助项目(2012104008-1)

摘　　要：目的：建立中成药中金胺O染色物的检测方法，对可能存在的化工染料金胺O进行筛查，并建立阳性样品中的含量测定方法。方法：采用HPLC法对中成药中的金胺O进行筛查，并采用HPLC-MS/MS二级质谱对阳性样品进行确认。质谱采用电喷雾正离子扫描（ESI＋），二级质谱全扫描模式（product ion mode），母离子m/z 268.1，子离子扫描范围m/z 20～300。在此基础上，采用高效液相色谱法对阳性样品中的金胺O进行含量测定。色谱条件：采用Phenomenex Gemini C18色谱柱（250 mm×4.6 mm，5 μm），以乙腈-0.05 mol·L^-1醋酸铵水溶液（冰醋酸调pH 4.5）（30：70）为流动相，流速1 mL·min^-1，检测波长432 nm。结果：采用HPLC法对94批次中成药进行筛查，并采用HPLC-MS/MS对可疑样品进行确认;有4批样品可检出金胺O;金胺O进样在0.00202～2.02 μg的范围内有良好的线性关系。阳性样品元胡止痛片、朱砂安神丸中金胺O的平均回收率（n=9）分别为101.6%（低、中、高3个浓度回收率分别为101.1%、101.2%和102.6%）和98.4%（低、中、高3个浓度回收率分别为99.7%、95.6%和99.9%）。4批阳性样品（2批元胡止痛片样品和2批朱砂安神丸样品），其含量方别为2.7 μg·片^-1（糖衣片）、1.7 μg·片^-1（糖衣片）、100.8 μg·g-1（水蜜丸）和252.6 μg·丸^-1（大蜜丸）。结论：本方法准确可靠，可作为元胡止痛片、朱砂安神丸中金胺O染色物的检测方法。Objective： To develop a method for detecting,screening and quantifying the possibly exiting auramine O in Chinese patent medicines. Methods： HPLC was used as the screening method of auramine O.The positive results of screening were confirmed by HPLC-MS/MS with ESI＋ ion source.The ion at m/z 268.1 was selected as the precursor ion for MS/MS analysis and the resulting product ion spectrum was recorded between m/z 20 and m/z 300.Based on those results,an HPLC method was developed for the qualification of auramine O in positive samples.A Phenomenex Gemini C18 （250 mm×4.6 mm,5 μm）column was adopted,the mixture of acetonitrile and 0.05 mol·L^-1 ammonium acetate（adjusted to pH 4.5 with glacial acetic acid）（30： 70）was used as the mobile phase,the flow rate was 1 mL·min^-1,and the detection wavelength was set at 432 nm. Results： The HPLC method was used for the screening of 94 batches of Chinese patent medicines.The suspected samples were confirmed by HPLC-MS/MS.Auramine O was detected from 4 batches of samples.Auramine O had considerable linear relationship in the range of 0.00202-2.02 μg.The average recoveries of auramine O in Yuanhu Zhitong tablets and Zhusha Anshen pills were 101.6%（101.1%,101.2%,and 102.6% for low,middle,and high concentrations respectively）and 98.4%（99.7%,95.6%,and 99.9% for low,middle,and high concentrations respectively）.The contents of auramine O in 4 batches of positive samples（2 batches of Yuanhu Zhitong tablets and 2 batches of Zhusha Anshen pills）were 2.7 μg per tablet（sugar coated tablets）,1.7 μg per tablet（sugar coated tablets）,100.8 μg·g-1 （water-honeyed pills）,and 252.6 μg per pill（big honeyed pills）,respectively. Conclusion： This method is accurate and reliable,and can be used as the detection method for auramine O in Yuanhu Zhitong tablets and Zhusha Anshen pills.

关 键 词：中成药 元胡止痛片 朱砂安神丸 金胺O 化工染料 高效液相色谱 液相色谱-质谱联用 安全监测 

分 类 号：R917[医药卫生—药物分析学]