水果和红茶中腈菌唑对映体残留的超高效合相色谱四极杆飞行时间质谱分析  

Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry

作　　者：张新忠[1,2] 赵悦臣[3] 罗逢健[1,2] 陈宗懋[1,2] 崔新仪[3] 周利[1,2] 楼正云[1,2] 

机构地区：[1]中国农业科学院茶叶研究所农产品质量安全研究中心,浙江杭州310008 [2]农业部茶叶产品质量安全风险评估实验室,浙江杭州310008 [3]天津农学院园艺园林学院,天津300384

出　　处：《分析测试学报》2016年第11期1376-1383,共8页Journal of Instrumental Analysis

基　　金：国家自然科学青年基金(21107137);国家茶叶产业技术体系(CARS-23);浙江省自然科学基金(Y3100259);中国农业科学院创新工程

摘　　要：采用超高效合相色谱四极杆飞行时间质谱,建立了手性农药腈菌唑对映体在苹果、葡萄和茶叶中的对映体拆分与残留分析方法。样品采用乙腈提取,Cleanert TPT或Pesti Carb柱净化,优化合相色谱条件将腈菌唑对映体进行分离,四极杆飞行时间质谱基质外标法定量测定。对合相色谱的影响因素进行了优化,确定最佳条件为：Chromega Chrial CCA色谱柱,流动相采用CO_2-异丙醇（95∶5）,流速2.0 m L/min,动态背压13.79 MPa,柱温30℃,柱后离子化辅助溶剂为含2 mmol/L甲酸铵的甲醇-水（1∶1）溶液。结果表明：在0.01~1.00 mg/L浓度范围内,标准曲线满足线性关系,相关系数在0.98以上;在0.005,0.025,0.25 mg/kg加标水平下,苹果和葡萄中腈菌唑对映体的平均回收率（n=6）为62.5%~103.0%,相对标准偏差均不大于9.9%,方法定量下限为0.005 mg/kg;在0.01,0.05,0.5 mg/kg加标水平下,红茶中腈菌唑对映体的平均回收率（n=6）为84.1%~86.4%,相对标准偏差均小于9.6%,方法定量下限为0.01 mg/kg。A separation and residue determination method for myclobutanil enantiomers in apple, grape and black tea was firstly developed by ultra performance convergence chromatography combined with quadrupole time - of - flight mass spectrometry （ UPC2 - QTOF/MS）. Samples were extracted with acetonitrile, purified with Cleaneert TPT or Cleanert PestiCarb solid-phase extraction（SPE） col- umns, and separated in the optimum condition of convergence chromatography, then analyzed by UPC2 - QTOF/MS with the matrix external standard method. All the influence factors of convergence chromatography（ chromatographic column, mobile phase modifier and proportion, column temperature, automated backpressure regulator, and post-column auxiliary solvent） were optimized. The best conditions were as iollows： ChromegaChrial CCA column with a mobile phase of CO2 - isopro- panol（95 ： 5）, a flow rate of 2.0 mL/min, an automated baekpressure regulator（ABPR） of 13.79MPa, a column temperature of 30 ℃, and a post-column auxiliary solvent of methanol - water（ 1 ： 1 ） containing 2 mmol/L ammonium formate. The results showed that the linear ranges of myclobutanil enantiomers were in the range of 0.01 - 1.00 mg/L, and the correlation coefficients were above 0. 98. The reeoveries of myclobutanil enantiomers at three spiked levels of 0. 005, 0. 025, 0.25 mg/kg in fruit matrix were in the range of 62.5% - 103.0% with relative standard deviations （ RS- Ds, n =6） not more than 9.9% , and the limits of quantitation （LOQ） of enantiomers were 0. 005 mg/kg. The recoveries of myelobutanil enantiomers at three spiked levels of 0.01, 0. 05, 0.5 mg/ kg in black tea matrix were 84. 1% - 86.4% with RSDs（n =6） less than 9.6% , and the LOQ for these two enantiomers were 0. 01 mg/kg. The method was rapid, convenient and reliable, and could meet the requirement for residue analysis.

关 键 词：手性对映体 残留分析 腈菌唑 超高效合相色谱 四极杆飞行时间质谱 

分 类 号：O657.63[理学—分析化学] S482.2[理学—化学]