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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,2.7μm)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1.1~3.3μg/m L;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。
OBJECTIVE To establish a series of health food products that illegally add 13 hypoglycemic chemicals (tolbutamide, glibenclamide, gliclazide, glipizide, gliquidone, glimepiride, HPLC, a rapid test method for the determination of alanine, endostatin, pioglitazone hydrochloride, pioglitazone hydrochloride, metformin hydrochloride, phenformin hydrochloride, buformin hydrochloride, and glareotide). Methods The chromatographic column CORTECS-C18 (100 mm × 4.6 mm, 2.7 μm) with high chromatographic performance was used for the rapid separation and the detection by diode array detector (PDA). The samples were extracted with methanol as the solvent, Tolbutamide, glyburide, gliclazide, glipizide, gliquidone, glimepiride, rosiglitazone maleate, Repaglinide, pioglitazone hydrochloride, metformin hydrochloride, phenformin hydrochloride, buformin hydrochloride, and glibenclamide. Results The chromatograms of thirteen hypoglycemic chemical constituents showed good resolution, wide linear range and good correlation with r2 ≥ 0.998 7. The precision of the method was expressed as RSD of 6 determinations, which was 0.6% -1.5% The recoveries ranged from 95.9% to 104.7%. The limits of quantification ranged from 1.1 μg / ml to 3.3 μg / ml. The RSDs for daytime precision ranged from 0.5% to 1.6% (n = 9). Sixteen batchs of chemical drugs were detected in 17 batches of glyceryl dietary supplements with the detection rate of 20%. Glyburide, phenformin hydrochloride, rosiglitazone maleate, glimepiride , Metformin hydrochloride, pioglitazone hydrochloride. Conclusion The method is versatile and easy to operate. It can be used as an effective method to illegally add 13 kinds of hypoglycemic chemical components in health food.