稳定同位素内标/超高压液相色谱-串联质谱法同时测定水果与豆芽中10种植物生长调节剂残留

建立了水果与豆芽中10种植物生长调节剂残留的超高压液相色谱-串联质谱(UPLC-MS/MS)分析方法。以酸化乙腈(1∶1 000,体积比)为提取液,样品经高速匀浆与超声辅助分散提取后,提取液采用固相萃取柱净化,甲醇-5 mmol/L乙酸铵溶液为流动相,梯度洗脱,电喷雾电离,正负离子扫描,多反应监测模式(MRM)检测,基质匹配同位素内标标准曲线定量。最优条件下,10种植物生长调节剂残留在0.1~50.0μg/L浓度范围内线性关系良好,相关系数(r2)均大于0.995,检出限为0.2μg/kg,平均回收率为52.4%~119.6%,相对标准偏差(RSD)均小于13%。该方法样品前处理简单、净化效果好,同位素内标的使用解决了基质效应及前处理过程中待测物损失造成定量结果不准确的问题,适用于大批量果蔬中多种植物生长调节剂的快速测定。

Simultaneous Determination of Ten Plant Growth Regulator Residues in Fruit and Bean Sprout by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Stable Isotope-labelled Internal Standards

A method for the determination of ten plant growth regulator residues in fruit and bean sprout by ultra performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) was established.The samples were extracted by the stirring and ultrasound using formic acid-acetonitrile (1 ∶ 1 000),and purified with the solid phase extraction column.The analytes were separated by using methanol-5 mmol/L ammonium acetate as mobile phase.The identifications were achieved by the electrospray ionization in positive and negative mode (ESI +/ESI-) using the multiple reaction monitoring(MRM).The quantifications were performed by the matrix matched isotope-labelled internal standards.Under the optimal experimental conditions,the calibration curves of ten analytes showed good linearities in the concentration range of 0.1-50.0 μg/L with correlation coefficients(r2) above 0.995.Recoveries were between 52.4％ and 119.6％ with RSDs less than 13.0％.The limits of detection were 0.2 μg/kg.The method had the advantages of simple pretreatment,good purification and low matrix effects,and was suitable for the rapid,high-throughput quantitative analysis of plant growth regulator residues in fruit and bean sprout.