Simultaneous and enantioselective determination of cis-epoxiconazole and indoxacarb residues in various teas, tea infusion and soil samples by chiral high performance liquid chromatography coupled with tandem quadrupole-time-of-flight mass spectrometry
Simultaneous and enantioselective determination of cis-epoxiconazole and indoxacarb residues in various teas, tea infusion and soil samples by chiral high performance liquid chromatography coupled with tandem quadrupole-time-of-flight mass spectrometry
复制标题
手性高效液相色谱-串联四极杆飞行时间质谱法同时对映选择性测定各种茶叶、茶汤和土壤样品中的顺式氟环唑和茚虫威残留量
DOI：
10.1016/j.chroma.2014.07.058
复制
发表时间：
2014-09-12
影响因子：
4.1
通讯作者：
Chen, Zongmao
中科院分区：
文献类型：
--
作者：
Zhang, Xinzhong;Luo, Fengjian;Chen, Zongmao
建立了一种同时测定茶叶、红茶浸液和土壤样品中顺氟环唑和茚虫威对映体的新方法。样品首先进行乙腈提取，然后使用实验室制备的弗罗里硅土/石墨化炭黑混合固相萃取（SPE）柱（用于不同的茶和土壤样品）和BondElut C-18-SPE柱（用于红茶浸泡液样品）进行净化。在手性固定相上使用高效液相色谱法（HPLC）在反相等度洗脱模式下进行分析物的分离，然后通过串联四极杆飞行时间质谱（Q-TOF/MS）检测。对移动的相组成、移动的相比例、流速、柱温和MS参数进行了优化，以达到高灵敏度和选择性、良好的峰形和令人满意的分离度。根据灵敏度、线性、准确度、精密度和基质效应评价了该方法的性能。在最佳条件下，对不同茶叶（绿色茶、红茶和普洱茶）、新鲜茶叶、土壤和红茶茶汤样品进行了低、中、高3个水平的加标，4种对映体的平均回收率为61.0%~ 129.7%，相对标准偏差（RSD）均小于17.1%。所有目标对映体的回归系数（R）均在0.9915或以上，基质匹配校准浓度范围为5.0 - 1000 μ g/L，线性良好。所有四种目标对映异构体的检测限（LOD）在不同的茶和土壤样品中为1.4 μ g/kg或更低，在红茶浸泡液中为0.05 μ g/kg或更低，而定量限（LOW）分别不超过5.0 μ g/kg和0.2 μ g/L。该方法简便可靠，已应用于真实的茶叶样品的筛选。该方法也被扩展到田间试验中的降解动力学和环境行为研究，为这些手性农药的可靠风险评估提供了额外的信息。(C)2014爱思唯尔有限公司版权所有。
A novel and sensitive method for simultaneous enantiomeric analysis of two pesticides-cis-epoxiconazole and indoxacarb in various teas, black tea infusion, and soil samples has been developed. The samples were initially subjected to acetonitrile extraction followed by cleanup using lab-made florisil/graphitized carbon black mixed solid phase extraction (SPE) column (for the different teas and soil samples) and a BondElut C-18-SPE column (for the black tea infusion samples). Separation of the analytes was performed on a chiral stationary phase using high performance liquid chromatography (HPLC) under a reversed-phase isocratic elution mode followed by tandem quadrupole time-of-flight mass spectrometry (Q-TOF/MS) detection. The mobile phase components, mobile phase ratios, flow rates, column temperatures, and MS parameters were all optimized to reach high sensitivity and selectivity, good peak shape, and satisfactory resolution. The performance of the method was evaluated based on the sensitivity, linearity, accuracy, precision, and matrix effects. Under optimal conditions, for the various teas (green tea, black tea, and puer tea), fresh tea leaf, soil and black tea infusion samples spiked at low, medium, and high levels, the mean recoveries for the four enantiomers ranged from 61.0% to 129.7% with most relative standard deviations (RSDs) being 17.1% or below. Good linearity can be achieved with regression coefficients (R) of 0.9915 or above for all target enantiomers, and matrix-matched calibration concentration ranging from 5.0 to 1000 mu g/L. The limits of detection (LODs) for all four target enantiomers were 1.4 mu g/kg or below in the different teas and soil samples and 0.05 mu g/kg or below in the black tea infusion, whereas the limits of quantification (LOW) for those did not exceed 5.0 mu g/kg and 0.2 mu g/L, respectively. The proposed method is convenient and reliable and has been applied to real tea samples screening. It has also been extended for studies on the degradation kinetics and environmental behaviors in the field trials, providing additional information for reliable risk assessment of these chiral pesticides. (C) 2014 Elsevier B.V. All rights reserved.