1. 中国农业科学院茶叶研究所农产品质量安全研究中心
2. 农业部茶叶产品质量安全风险评估实验室
3. 天津农学院园艺园林学院
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张新忠, 赵悦臣, 罗逢健, 等. 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[J]. 分析测试学报, 2016,35(11):1376-1383.
Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry[J]. 2016,35(11):1376-1383.
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PestiCarb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:ChromegaChrial CCA色谱柱,流动相采用CO2-异丙醇(95∶5),流速2.0mL/min,动态背压13.79MPa,柱温30℃,柱后离子化辅助溶剂为含2mmol/L甲酸铵的甲醇-水(1∶1)溶液。结果表明:在0.01~1.00mg/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0.005,0.025,0.25mg/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0.005mg/kg;在0.01,0.05,0.5mg/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0.01mg/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) columns,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 follows: ChromegaChrial CCA column with a mobile phase of CO2-isopropanol(95∶5),a flow rate of 2.0mL/min,an automated backpressure regulator(ABPR) of 13.79MPa,a column temperature of 30℃,and a post-column auxiliary solvent of methanol-water(1∶1) containing 2mmol/L ammonium formate. The results showed that the linear ranges of myclobutanil enantiomers were in the range of 0.01-1.00mg/L,and the correlation coefficients were above 0.98.The recoveries 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(RSDs,n=6) not more than 9.9%,and the limits of quantitation(LOQ) of enantiomers were 0.005mg/kg.The recoveries of myclobutanil enantiomers at three spiked levels of 0.01,0.05,0.5mg/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 0.01mg/kg.The method was rapid,convenient and reliable,and could meet the requirement for residue analysis.
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
chiral enantiomersresidual analysismyclobutanilultra performance convergence chromatography(UPC2)quadrupole time-of-flight mass spectrometry(QTOF/MS)
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