采用反相高效液相色谱法测定降糖类保健食品非法添加降糖化学药品检验方法的研究

Identification of eleven components of diabetes medicine added illegally to health products by HPLC

目的建立同时测定降糖类保健食品中非法添加盐酸二甲双胍、盐酸苯乙双胍、甲苯磺丁脲、格列吡嗪、格列齐特、马来酸罗格列酮、盐酸吡格列酮、格列本脲、格列美脲、格列喹酮和瑞格列奈11种化学药品含量的反相高效液相法。方法采用Agilent Eclipse Plus C18色谱柱(250mm×4.6mm,5μm),以甲醇(A)-20mmol乙酸铵水溶液(B)为流动相,梯度洗脱(0～4min:30%A;4～10min:30%A→50%A;10～30min:50%A→70%A;30～35min:70%A;35～40min:70%A→85%A;40～45min:85%A;45～50min:85%A→30%A;50～60min:30%A),流速为0.8mL/min,紫外检测波长230nm。柱温35℃。结果在50min内可同时分离检测11种成分,11种对照品的浓度在1～50μg/mL范围内与峰面积呈良好的线性关系,均r>0.9995,平均回收率均在96.0%～104.0%。结论该方法简便、准确、稳定、重现性好,可用于该类保健食品中非法添加化学药品的定量检测。

【Objective】To establish a method for identification of eleven components of diabetes medicine added illegally to health products by HPLC.【Methods】 The analysis was performed with a Agilent Eclipse Plus C18 column（250 mm×4.6 mm,5 μm） and a mobile phase of methanol（A）-0.02 mol/L ammonium acetate（B） with gradient elution[0～4 min：30% A;4～10 min：30% A→50% A;10～30 min：50% A→70% A ;30～35 min：70% A;35～40 min：70% A→85% A;40～45 min：85% A;45～50 min：85% A→30% A;50～60 min：30% A].The flow rate was 0.8 mL/min and column temperature was 35 ℃.The detection wave length was set 230 nm.【Results】The eleven ingredient can be separated in 50 min.The linear range of eleven componts were 1.00～50.00 μg/mL（r 0.9994）.The recovery rates were between 96.0% and 104.0%.【Conclusion】The method is convenient and accurate.It suitable for the quantitative determination of illegal additives in health food.