液相色谱-串联质谱法检测蔬菜中氯吡脲残留量的前处理研究

Pre-treatment of determination of forchlorfenuron residues in vegetables by liquid chromatography-tandem mass spectrometry

中文关键词:  前处理  氯吡脲  液相色谱-串联质谱法  蔬菜

英文关键词:pre-treatment  forchlorfenuron  liquid chromatography-tandem mass spectrometry  vegetables

中文摘要:

      目的 利用正交实验构建一种液相色谱-串联质谱法检测蔬菜中氯吡脲残留量的前处理方法。方法 通过加标回收率的比较, 从二氯甲烷、乙酸乙酯、丙酮、乙腈中选择合适的提取溶剂和提取方式; 选取氨基固相萃取柱为净化柱; 从甲醇、二氯甲烷、甲醇-二氯甲烷等中选择适合的洗脱溶剂。使用20 mL乙腈体系对样品进行30 min提取, 经氨基柱净化, 二氯甲烷为淋洗液, 甲醇为洗脱剂, 45 ℃氮吹浓缩富集, 甲醇溶液定容过滤后测定。结果 通过加标回收率和精密度实验, 结果表明平均加标回收率为91%~116%和相对标准偏差(RSD)为1.6%~5.6%。结论 该方法简单、实用、快速, 具有较高的准确度和重复性, 可用于蔬菜中氯吡脲的残留量测定的前处理。

英文摘要:

      Objective To establish a pre-treatment method for the determination of forchlorfenuron residues in vegetables by liquid chromatography tandem mass spectrometer. Method According to comparison of the standard recovery rates, the right extraction solvent and method were chosen from methylene chloride, ethyl acetate, acetone and acetonitrile with amino solid-phase extraction column as spin column. Suitable solvent elution was chosen from methanol, dichloromethane and methanol-dichloromethane. The sample was extracted by 20 mL acetonitrile for 30 min, cleaned up by solid-phase extraction NH2 column, eluted by methylene chloride, enriched by nitrogen at 45 ℃ , constant-volumed by methanol, filtered and detected by instrument. Results According to the average recoveries and precision experiments, the result showed that the average recoveries were 91%~116% and relative standard deviation(RSD )was 1.6%~5.6%.Conclusion This method is simple, practical, quick with high accuracy and repeatability, and can be used as a pre-treatment method for the determination of forchlorfenuron residues in vegetables.