摘要
目的建立液质联用法测定降糖类药品和保健食品中非法添加盐酸丁二胍的定性及定量方法。方法液质联用定性筛查选用ThermoHypersil ODS-2(2.1mm×150mm,5μm)柱,以甲醇-0.01mol.L-1乙酸铵(20∶80)为流动相,流速0.3mL.min-1。经液质联用筛查为阳性的样品用液相色谱进行含量测定,选用Thermo Hypersil ODS-2(4.6mm×150mm,5μm)柱,以甲醇-离子对试液(庚烷磺酸钠0.5056g,加三乙胺1.4mL,加水至1000mL,用磷酸调节PH至3.5±0.05)为流动相梯度洗脱,检测波长235nm,流速1mL.min-1。通过对比对照品与供试品的色谱及质谱行为,对降糖类药品和保健食品中非法添加的盐酸丁二胍进行定性鉴别和定量测定。结果本方法能够在10min内快速检测降糖类药品和保健食品中是否非法添加盐酸丁二胍化学药物。在从市场上抽样的153批降糖类药品和保健食品中,有5批样品检测出非法添加了盐酸丁二胍。结论该方法快速、准确、灵敏度高,可作为分析检测降糖类药品和保健食品中非法添加盐酸丁二胍的有效方法 。
:OBJECTIVE To develop a HPLC-MS-MS method for the identification of buformin illegally added into hypoglycemic drugs and health-care food. METHODS The liquid chromatography-quadrupole mass spectrome- try method was used to detect the buformin illegally added into the hypoglycemic drugs and health-care food accord- ing to comparising the chromatographic behavior and mass spectral data with reference substances. RESULTS This method can screen buformin added illegally in drugs and health-care food within 10 minutes. Buformin was detected in five health care food from one hundred and fifty-three samples. CONCLUSION The method is rapid and sensi- tive and can he used to detect the illegal hypoglycemic drugs and health-care food.
出处
《海峡药学》
2013年第7期76-78,共3页
Strait Pharmaceutical Journal
基金
2010年广东药检系统药品监督抽验课题(ZA20101511)
关键词
降糖类药品和保健食品
非法添加
盐酸丁二胍
液质联用
Hypoglycemic drugs and health-care food
Illegally added
Buformin
Liquid chromatographic-quadrupole mass spec-trometry