[关键词]
[摘要]
目的 建立保健食品中非法添加13种降糖性化学成分(甲苯磺丁脲、格列本脲、格列齐特、格列吡嗪、格列喹酮、格列美脲、马来酸罗格列酮、瑞格列奈、盐酸吡格列酮、盐酸二甲双胍、盐酸苯乙双胍、盐酸丁二胍、格列波脲)的HPLC快速检测方法。方法 以高色谱性能的实心核颗粒色谱柱CORTECS-C18(100 mm×4.6 mm,2.7 μm)快速分离,二极管阵列检测器(PDA)检测,进行定性定量检测分析,样品以甲醇为溶剂超声提取,在10 min内同时检测添加在保健食品中的甲苯磺丁脲、格列本脲、格列齐特、格列吡嗪、格列喹酮、格列美脲、马来酸罗格列酮、瑞格列奈、盐酸吡格列酮、盐酸二甲双胍、盐酸苯乙双胍、盐酸丁二胍、格列波脲13种化学成分。结果 13种降糖化学成分色谱检测的分离度好,线性范围宽,相关性好,r2≥0.998 7;方法精密度以6次测定值的RSD表示,为0.6%~1.5%;方法回收率用3个质量浓度进行添加实验,回收率为95.9%~104.7%;定量限为1.1~3.3 μg/mL;日间精密度的RSD为0.5%~1.6%(n=9)。86批降糖类保健食品中检出17批添加化学药,检出率为20%;样品中检出了格列本脲、盐酸苯乙双胍、马来酸罗格列酮、格列美脲、盐酸二甲双胍、盐酸吡格列酮。结论 本方法通用性强,操作简单、快捷,可作为保健食品中非法添加13种降糖化学成分的有效检测方法。
[Key word]
[Abstract]
Objective To develop an HPLC method with solid nuclear particle chromatographic column to determine 13 anti-diabetic drugs illegally added in health food. Methods The analysis was performed by an HPLC system of Waters e2695, with Cortecs-C18 (100 mm × 4.6 mm, 2.7 μm) column. PDA was performed to identify and quantify tolbutamide, glibenclamide, gliclazide, glipizide, gliquidone, glimepiride, rosiglitazone, repaglinide, pioglitazone hydrochloride, metformin, phenformin, buformin hydrochloride, and glibomuride, which were extracted with methanol by ultrasonic. Results Thirteen linear calibration curves were obtained with r2 ≥ 0.998 7. The precision of the method was shown by RSD (n = 6) ranged from 0.6% to 1.5%. The recoveries were determined at three concentrations and ranged from 95.9% to 104.7%. The ranges of LLOQ were from 1.1 μg/mL to 3.3 μg/mL and the RSDs (n = 9) of inter-day precision were from 0.5% and 1.6%. Seventeen batches in 86 antidiabetic health foods were added the chemicals with positive rate of 20%. The glibenclamide, buformin hydrochloride, rosiglitazone, glimepiride, metformin, and pioglitazone hydrochloride were determined.Conclusion The method is specific, simple, and fast to detect 13 anti-diabetic drugs illegally added in health food.
[中图分类号]
[基金项目]
浙江省食品药品监管系统科技计划项目(SP201709)