QuEChERS-超高效液相色谱-串联质谱法快速测定3种叶菜中矮壮素和丙环唑残留

Fast Determination of Chlormequat and Propiconazole Residues in Three Leafy Vegetables by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了菜心、芥蓝和小白菜中矮壮素和丙环唑残留的分析方法。以QuEChERS法进行样品前处理,采用含1%HAc的乙腈溶液提取,无水MgSO4、C18及PSA吸附剂净化,超高效液相色谱-串联质谱(UPLC-MS/MS)法测定。对提取溶剂、吸附剂和色谱柱的选择进行了研究探讨。结果表明矮壮素在1~1 000μg/L、丙环唑在1~500μg/L浓度范围内均有良好的线性关系。矮壮素和丙环唑的检出限分别为0.1μg/kg和0.01μg/kg;在0.010、0.10和0.50mg/kg 3个添加浓度水平下,菜心、芥蓝和小白菜中矮壮素和丙环唑回收率为75.0%~96.2%;相对标准偏差为0.9%~8.3%;方法定量限为最低添加浓度0.010mg/kg。该方法快速、简便、准确,满足叶菜中矮壮素和丙环唑残留分析的要求。

An analytical method was developed for the determination of chlormequat and propiconazole residues in three leafy vegetables including flowering Chinese cabbage,Chinese kale and pak-choi. Target compounds were extracted by acetonitrile containing 1% acetic acid and cleaned up by magnesium sulfate anhydrous, C18 and PSA adsorbents, then detected with ultra performance liquid chromatography-tandem mass spectrometry. The optimization of extraction solvent, adsorbent and chromatographic column was studied. The linear ranges of chlormequat and propiconazole were 1-1 000 μg/L and 1- 500 μg/L, respectively with good linear relationship. Limit of detection of chlormequat was 0.1 /ag/kg while 0.01 μg/kg for propiconazole. Recoveries at three spiked levels of 0. 010,0.10 and 0.50 mg/kg were ranged from 75.0% to 96.2% with relative standard deviations from 0. 9% to 8.3 %. Limit of quantification of both chlormequat and propiconazole was 0.010 mg/kg. The method is quick, easy and accurate which can meet the requirements for the determination of chlormequat and propiconazole residues in leafy vegetables.