柱前衍生化-HPLC-MS/MS法测定启脾丸中掺假蜂蜜

Determination of Syrup Adulterated Honey in Qipiwan by Precolumn Derivatization-HPLC-MS/MS

建立了启脾丸中掺假蜂蜜的测定方法。供试品经活性炭固相萃取柱处理,采用1-苯基-3-甲基-5-唑啉酮衍生化试剂对其衍生化,以麦芽六糖和麦芽七糖的衍生产物为特征标志物,采用Waters CORTECS色谱柱和乙腈-0.1%甲酸水为流动相梯度洗脱,应用高效液相色谱-质谱进行分析。结果表明,天然蜂蜜不含麦芽六糖和麦芽七糖,麦芽糖浆、果葡糖浆、大米糖浆、木薯糖浆、甜菜糖浆以及掺假炼蜜含有大量麦芽六糖和麦芽七糖,结果发现5批启脾丸发现糖浆掺假蜂蜜投料。该试验所建方法结果可靠,灵敏度高,可为蜂蜜及含蜂蜜中药制剂的专项治理提供有力的技术支持。

A method was established for inspecting adulterated honey in Qipiwan.The test sample was treated by activated carbon solid phase extraction column,and 1-phenyl-1-phenyl-2-pyrazolin-5-one(PMP)derivatization reagent was used.Mobile phase gradient elution with a Waters CORTECS column and acetonitrile-0.1%formic acid water.The selection of derivatives of maltohexaose and maltoheptaose as characteristic markers was analyzed by high performance liquid chromatography-mass spectrometry(HPLC-MS/MS).The results showed natural honey did not contain maltohexaose and maltoheptaose,maltose syrup,fructose syrup,rice syrup,tapioca syrup,beet syrup and adulterated honey contain a large amount of maltohexaose and maltoheptaose,and 5 batches of Qipiwan were adulterated with syrup.The method had reliable results and high sensitivity,and it could provide powerful technical support for the special treatment of honey and honeycontaining traditional Chinese medicine preparations.