多壁碳纳米管滤过型净化柱净化-超高效液相色谱/串联质谱法同时测定生姜中的涕灭威及其代谢物

Analysis of aldicarb and its metabolites in ginger using ultra performance liquid chromatography-tandem mass spectrometrycoupled with multiplugfiltration clean upwith multiwalled carbon nanotubes

建立了多壁碳纳米管滤过型净化柱净化-超高效液相色谱/串联质谱联用技术同时测定生姜中涕灭威及其代谢物的分析方法。生姜样品经乙腈提取后，用多壁碳纳米管滤过型净化柱进行2次反复抽提净化，净化液用氮气吹干，用乙腈-水（5∶95，v / v）溶解，采用正离子多反应监测（MRM）模式进行分析，外标法定量。结果表明：涕灭威、涕灭威砜及涕灭威亚砜在0.5~200μg / L 浓度范围内呈线性，其相关系数（ r2）均大于0.99；在2、20、200μg / kg 添加水平下，回收率为71.4％~89.8％，相对标准偏差范围为0.7％~13.2％；3种目标物的定量限为1.0~2.0μg / kg。本方法操作简单，灵敏度、准确度和精密度均满足农药多残留检测技术的要求，适用于生姜中涕灭威及其代谢物残留的快速测定。

A simple and rapid pretreatment procedure was developed for the simultaneous determination of aldicarb and its metabolites,aldicarb sulfone and aldicarb sulfoxide,in ginger. The samples were extracted with acetonitrile,and then cleaned up with multiplug filtration using multiwalled carbon nanotubes（ MWCNTS）. The eluate was dried with nitrogen gas at room temperature,and redissolved in an acetonitrile-water（5 ∶95,v / v）mixture,then quanti-fied by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry （ UPLC-ESI-MS / MS ） operated in positive multiple reaction monitoring （MRM）mode. A linear relationship was achieved in the range of 0. 5 - 200 μg / L for the peak areas to the mass concentrations of the target compounds with the linear correlation coeffi-cients（r2 ）higher than 0. 99. The recoveries at three spiked levels of 2,20 and 200 μg / kg were in the range from 71. 4% to 89. 8% with the relative standard deviations（ RSDs,n = 6）from 0. 7% to 13. 2% under the selected conditions. The limits of quantification（ LOQ,S / N = 10）of aldicarb,aldicarb sulfone,and aldicarb sulfoxide in ginger were 1. 0,2. 0 and 1. 0 μg / kg, respectively. The results demonstrate that the developed method is rapid,cost-effective,and can meet the requirements of the multiple pesticide residue analysis. The method is applicable to determine aldicarb and its metabolites in ginger.