LC-MS快速检测降糖类中成药中14种非法添加化学药物

Rapid Detection of 14 Chemical Drugs Illegally Added in Antidiabetic Traditional Chinese Medicine by LC-MS

关键词:  液质联用法  降糖  中成药  非法添加

Key words:  LC-MS  antidiabetic  traditional Chinese medicine  illegal addition

摘要:

目的 建立一种降糖类中成药中非法添加的14种化学成分（伏格列波糖、阿卡波糖、维达列汀、氯磺丙脲、醋磺己脲、西他列汀、妥拉磺脲、达格列净、那格列奈、莫格他唑、卡格列净、曲格列酮、GW501516、环格列酮）的LC-MS检测方法。方法 样品经甲醇超声提取后，采用资生堂CAPCELL-PAK C₁₈（4.6 mm×150 mm，5 μm）色谱柱分离，以甲醇-0.01 mol·L^-1乙酸铵溶液为流动相进行梯度洗脱，流速0.5 mL·min^-1。采用离子阱质谱（ion trap mass spectrometry，ITMS）作为检测器，电喷雾离子源（ESI），正负离子扫描方式，以一级全扫描模式和二级全扫描模式检测14种降糖类药物。通过比较供试品和对照品的色谱图及质谱图，对供试品中非法添加的化学药物进行定性分析。结果 14种化合物色谱峰分离良好，最低检出限为0.05~3.5 mg·kg^-1。30批样品中，3批检出卡格列净，1批检出那格列奈。结论 该方法灵敏度高，专属性强，操作简单高效，可用于降糖类中成药中非法添加的14种化学药物的快速检测。

Abstract:

OBJECTIVE To establish a rapid method for qualitative determination of 14 chemical drugs(including voglibose, acarbose, vildagliptin, chlorpropamide, acetohexamide, sitagliptin, tolazamide, dapagliflozin, nateglinide, muraglitazar, canagliflozin, troglitazone, GW501516, ciglitazone) illegally added into antidiabetic traditional Chinese medicines by LC-MS. METHODS Samples were separated on a SHISEIDO HPLC CAPCELL-PAK C₁₈ column(4.6 mm×150 mm, 5 μm) after ultrasonic extracted by methanol with the mobile phase consisted of methanol-0.01 mol·L^-1 ammonium acetate solution by gradient elution. The flow rate was 0.5 mL·min^-1. Ion trap mass spectrometry(ITMS), electrospay ionization source(ESI) and positive and negative ion scanning were adopted to analyze 14 antidiabetic chemicals with full scan MS and full scan MS² modes. The qualitative analysis of 14 antidiabetic chemical drugs was performed by comparing the chromatograms and mass spectrograms of the reference substances and samples. RESULTS The 14 compounds were well separated under the selected LC-MS condition. The limits of detection were all in the range of 0.05-3.5 mg·kg^-1. Out of 30 batches of samples, 3 samples contained canagliflozin and 1 sample contained nateglinide. CONCLUSION The method is simple, sensitive and rapid in the detection of chemical drugs illegally added into antidiabetic traditional Chinese medicines.