超高效液相色谱串联质谱法测定豆芽中4－氯苯氧乙酸的含量
Determination of 4-Chlorophenoxyacetic Acid in Bean Sprout by UPLC-MS/MS
史晓磊1
作者信息
- 1. 上海德诺产品检测有限公司，上海200436
- 折叠
摘要
[目的]采用超高效液相色谱串联质谱法建立豆芽中4－氯苯氧乙酸的定性定量分析方法。[方法]样品经0．01 mol／L氢氧化钠溶液提取，Oasis HLB固相萃取小柱净化，C18色谱柱分离，乙腈－0．1％甲酸水溶液为流动相，采用电喷雾离子源多反应监测模式下液相色谱串联质谱法检测，基质曲线外标法定量。[结果]在最佳检测条件下，4－氯苯氧乙酸在20～500μg／L线性关系良好，相关系数为0．9981，检出限（S／N＝3）为20μg／kg。在加标水平为20、60、100μg／kg时的平均加标回收率分别为87．62％、102．10％和100．00％，其相对标准偏差（RSD）分别为3．48％、4．92％和6．59％。[结论]该方法具有灵敏度高、准确度和稳定性良好、操作简捷等的特点，能够满足残留分析的要求。
Abstract
Objective] To establish a qualitative and quantitative analysis method for 4-chlorophenoxyacetic acid in bean sprout by ultra per-formance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).[Method] The sample was extracted with 0.01 mol/L sodium hydroxide solution, and cleaned up with Oasis HLB.The separations were performed on a C18 column, with a mobile phase of 0.1% formic acid aqueous solution-acetonitrile and detected by positive-ion electrospray ionization mode and multi-reaction monitoring ( MRM) mode.[ Re-sult] Under the optimal test condition, 4-chlorophenoxyacetic acid showed good linear relationship within the range of 20 -500 μg/L, with correlation coefficient of 0.998 1.The limit of detection(S/N=3) was 20.0 μg/kg.The average recovery rates at three spiked levels of 20, 60, 100 μg/kg were 87.62%, 102.10% and 100.00%, respectively.The relative standard deviations (RSD) were 3.48%、4.92%and 6. 59%, respectively.[ Conclusion] This method had the characteristics of high sensitivity and accuracy, which can meet the requirement of re-tention analysis.
关键词
超高效液相色谱串联质谱法(UPLC-MS/MS)/固相萃取(SPE)/豆芽/4-氯苯氧乙酸Key words
UPLC-MS/MS/Solid phase extraction/Bean sprout/4-Chlorophenoxyacetic acid引用本文复制引用
出版年
2016
国家科技期刊平台
NSTL
维普
万方数据