CAJ | 학술논문

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。
건립료다벽탄납미관려과형정화주정화-초고효액상색보/천련질보련용기술동시측정생강중체멸위급기대사물적분석방법。생강양품경을정제취후，용다벽탄납미관려과형정화주진행2차반복추제정화，정화액용담기취간，용을정-수（5∶95，v / v）용해，채용정리자다반응감측（MRM）모식진행분석，외표법정량。결과표명：체멸위、체멸위풍급체멸위아풍재0.5~200μg / L 농도범위내정선성，기상관계수（ r2）균대우0.99；재2、20、200μg / kg 첨가수평하，회수솔위71.4％~89.8％，상대표준편차범위위0.7％~13.2％；3충목표물적정량한위1.0~2.0μg / kg。본방법조작간단，령민도、준학도화정밀도균만족농약다잔류검측기술적요구，괄용우생강중체멸위급기대사물잔류적쾌속측정。
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.