Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry
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Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry
Vol. 35, Issue 11, Pages: 1376-1383(2016)
作者机构:
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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Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry. [J]. 35(11):1376-1383(2016)
DOI:
Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry. [J]. 35(11):1376-1383(2016)DOI:
Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry
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.
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
Keywords
chiral enantiomersresidual analysismyclobutanilultra performance convergence chromatography(UPC2)quadrupole time-of-flight mass spectrometry(QTOF/MS)
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