一种快速筛查和确定保健品中11种降糖类药物的检测方法

采用高效液相色谱一离子阱飞行时间串联高分辨质谱对于保健品中降糖类药物共11种成分进行快速筛查、定性识别和准确定量。样品经含甲醇溶液超声提取，提取液经OuEChERS吸附剂净化，以C18色谱柱（150mm×2．0mm，3．0μm）分离，5mmol／I。乙酸铵溶液和0．5％甲酸乙腈为流动相梯度洗脱，正离子模式扫描。结果表明，11种化合物在2～1000μg／L范围内呈良好的线性相关性，相关系数均大于0．991。保健品样品中各化合物的定量限（以信噪比≥10计）分别为2．0～5％g／kg。在低、中、高3个添加水平下，各化合物的平均回收率为72．3％～118．1％，相对标准偏差（RSD）为0．5％～8．4％。该方法利用精确质量数匹配和自建标准谱库检索，实现快速筛查，并使用多级特征碎片离子进行确证，具有简便、快速、高效、准确等优点，适用于保健食品中降压降糖类药物的快速筛查和测定。

A detection method for rapid screening and confirmation of 11 antidiabetic drugs in health products

A method was developed for the screening and confirmation and quantification of 11 antidiabetic drugs in healthy foods by high performance liquid chromatography ion trap time of flight tandem mass spectrometry（HPLC-IT-TOF-MS）. The analytes in the sample were ex- tracted with methanol and the extract was purified with the mixed QuEChERS sorhents. In the chromatographic analysis,the 11 antidiabetic drugs were separated on a C18 column with the gradient elution using the mobile phases of acetonitrile and water containing 0.5 % acetic acid. The mass analyzer was performed in positive modes in one injection. The results showed that the line arranges of the 11 compounds were 2--1000/g/L with the correlation coefficients above 0. 991 and the limits of quantification（LOQ,S/N≥10）were2.0-50.0/μg/kg for capsuleand oral solution,respectively. The method validation was carried out at three spiked levels, and the recoveries were 72. 3%-118. 1% with the relative standard deviations（RSDs） of 0.5%-8.4 %. The screening of analytes was performed by precision mass matching and li- brary searching. These condary fragmention spectra were employed to the confirmation. This method is simple, fast, reliable, and can be applied to the simultaneous screening and determi- nation of hormones in health foods.