论文部分内容阅读
目的建立HPLC-MS/MS方法检测中药及保健品中非法添加的11种降糖类化学药物。方法采用Phenomenex C18(4.6 mm×250 mm,5μm)色谱柱,梯度洗脱:流动相A为0.1%甲酸溶液(用氨水调节pH值至3.2),流动相B为乙腈,检测波长为230 nm,流速为1 mL.min-1(分流比为4∶1)。选择正离子全扫描方式检测,扫描范围:50~1 000m/z。电喷雾参数:雾化器压力276 kPa,干燥气(N2)温度350℃,流速9.0 L.min-1,静电喷雾电压3 200 V,碰撞电压2 V。结果在本色谱条件下,11种临床常用的降糖药均有很好的分离。二甲双胍、苯乙双胍、罗格列酮、盐酸吡格列酮、格列吡嗪、甲苯磺丁脲、格列奇特、格列本脲、格列美脲,格列喹酮,瑞格列奈检测限均在1~25 ng之间。结论本法简便准确,可作为保健品及中成药中非法添加降糖化学成分的快速筛查方法 。
Objective To establish an HPLC-MS / MS method for the determination of 11 hypoglycemic drugs illegally added to traditional Chinese medicine and health products. Methods The mobile phase A was a 0.1% formic acid solution (adjusted to pH 3.2 with aqueous ammonia) using a Phenomenex C18 (4.6 mm × 250 mm, 5 μm) column. The mobile phase B was acetonitrile and the detection wavelength was 230 nm. The flow rate was 1 mL.min-1 (split ratio 4: 1). Select positive ion full scan detection, scanning range: 50 ~ 1 000m / z. Electrospray parameters: atomizer pressure 276 kPa, dry gas (N2) temperature 350 ℃, flow rate 9.0 L.min-1, electrostatic spray voltage 3 200 V, collision voltage 2 V. Results Under the chromatographic conditions, 11 commonly used hypoglycemic agents were well separated. Metformin, phenformin, rosiglitazone, pioglitazone hydrochloride, glipizide, tolbutamide, glibenclamide, glibenclamide, glimepiride, gliquidone and repaglinide Between 1 and 25 ng. Conclusion This method is simple and accurate and can be used as a rapid screening method for illegally adding chemical components of hypoglycemia in health products and proprietary Chinese medicines.