根痛平胶囊中非法添加染色物方法的建立  

Determination Method for Illegally Added Dyes to Gentongping Capsules

作　　者：杨晓 殷世宁 邱学伟 张春辉 Yang Xiao;Yin Shining;Qiu Xuewei;Zhang Chunhui(Qingdao Food and Drug Inspection Institute,Shandong Qingdao 266071,China)

机构地区：[1]青岛市食品药品检验研究院,山东青岛266071

出　　处：《中国药师》2020年第5期996-1000,共5页China Pharmacist

摘　　要：目的:建立一种用于快速检测中药材、中成药及保健品中非法添加的14种黄色系、橙色系、红色系染色物的超高效液相色谱(UPLC)及液相色谱-质谱(LC-MS)方法,并用于根痛平胶囊的筛查。方法:采用UPLC检测,Dikma Endevaorsil C18(100 mm×2.1 mm,1.8μm)色谱柱,以乙腈-0.02 mol·L-1乙酸铵溶液为流动相,梯度洗脱,检测波长分别为426,484,510 nm。采用LC-MS/MS法进行专属性确证,色谱柱:Waters ACQUITY UPLCTM BEH C18(50 mm#2.1 mm,1.7μm);以乙腈-0.02 mol·L-1乙酸铵溶液为流动相,梯度洗脱;柱温:30℃;流速:0.2 ml·min-1;进样量:10μl;扫描方式:ESI+;检测方式:多反应监测(MRM)模式。结果:14种染色物得到良好的分离效果,线性范围为2.0~30.0μg·ml-1,线性相关系数均大于0.9880,检测限在0.5~2.9μg·g-1之间,加样回收率为94.8%~98.4%,RSD为1.2%~3.3%(n=9)。244批次样品中有2批次检出柠檬黄、日落黄、胭脂红3种染色物。结论:本试验建立的非法染色物筛查方法准确、简便、可靠、选择性强,可快速、有效地检测根痛平胶囊中的非法染色物。Objective:To develop a UPLC-MS method for the rapid detection of 14 types of yellow,orange and red systems illegally added to Chinese herb medicines,Chinese patent medicines and health supplements,and supply the method to the screen of Gentongping capsules.Methods:Using UPLC for testing,a Dikma Endevaorsil C18(100 mm×2.1 mm,1.8μm)column was used.Gradient elution was conducted using the mobile phase consisting of acetonitrile and 0.02 mol·L-1 ammonium acetate at a flow rate of 1.0 ml·min-1.The detection wavelengths were set at 426,484 and 510 nm.An LC-MS/MS method was used to confirm the specificity.The chromatographic column was Waters ACQUITY UPLCTM BEH C18(50 mm×2.1 mm,1.7μm),and gradient elution was performed with acetonitrile-0.02 mol·L-1 ammonium acetate solution as the mobile phase.The column temperature was 30℃,the flow rate was 0.2 ml·min-1,and the injection volume was 10μl.The scanning mode was ESI+,and the detection mode was MRM.Results:The calibration curves of the fourteen dyes showed good linearity within the range of 2.0-30.0μg·ml-1 and the correlation coefficients were all above 0.9880.The lower limits of determination for fourteen dyes in the samples were between 0.5 and 2.9μg·g-1.The average recoveries for three concentration levels ranged from 94.8%-98.4%with the RSDs from 1.2%to 3.3%(n=9).Lemon yellow,sunset yellow and carmine were detected out in 2 samples in all 244 tested samples.Conclusion:The established method is selective,sensitive and accurate,which is suitable for the supervision and determination of fourteen illegal added dyes in Gentongping capsules.

关 键 词：非法染色 超高效液相色谱 液相色谱-质谱 根痛平胶囊 柠檬黄 日落黄 胭脂红 

分 类 号：R927.1[医药卫生—药学]