液相色谱–串联质谱法测定水果及其制品中氯吡脲残留量

建立了液相色谱–三重四极杆串联质谱测定水果及其制品中氯吡脲的方法。样品经乙腈提取,氨基固相萃取小柱净化后,用ZORBAX Extend-C18柱(150 mm×2.1 mm,5μm)分离,以甲醇–水为流动相等度洗脱,采用多反应监测正离子模式检测,外标法定量。氯吡脲的质量浓度在4.0~200.0 ng/m L范围内线性良好,相关系数大于0.999,在5.0,10.0,20.0μg/kg 3个添加水平下,氯吡脲的平均加标回收率为86%~92%,测定结果的相对标准偏差为5.3%~7.6%(n=5),方法定量下限为2.0μg/kg。方法灵敏度高,操作简便,定量准确,可满足梨、柑桔、黄桃等水果及其罐头制品中氯吡脲残留的检测与确证需要。

Determination of Forchlorfenuron Residues in Fruits and Fruit Products by LC-MS/MS

A method for determination of forchlorfenuron residues in fruits and fruit products was established by liquid chromatography–tandem mass spectrometry(LC–MS/MS). After being extracted by acetonitrile, the sample was cleaned up by solid-phase extraction NH2 column. The separation of compounds was carried on a ZORBAX Extend-C18 column(150 mm×2.1 mm, 5 μm) by an isocratic elution using methanol–water as mobile phase. The analyte was detected by tandem mass spectrometry under multiple reaction monitoring mode with positive electrospray ionization. The forchlorfenuron was quantified by external standard method. Under the optimal conditions, the calibration curve showed a good linearity over the concentration of forchlorfenuron in the range of 4.0–200.0 ng/mL with a correlation coefficient more than 0.999. The average recoveries from spiked samples at three concentration levels of 5.0, 10.0, 20.0 μg/kg ranged from86%–92% with the relative standards deviations of 5.3%–7.6%(n=5), the limit of quantitation was 2.0μg/kg. The method is simple and suitable for the determination and confirmation of forchlorfenuron in pear, orange and yellow peach or their canned products.