|
| Determination of Myclobutanil Enantiomers Residues in Fruit and Black Tea Samples by Ultra Performance Convergence Chromatography Quadrupole Time-of-Flight Mass Spectrometry |
| |
| View Full Text Download reader |
| DOI： |
| KeyWord:chiral enantiomers residual analysis myclobutanil ultra performance convergence chromatography(UPC2) quadrupole time-of-flight mass spectrometry(QTOF/MS) |
| Author | Institution |
| ZHANG Xin-zhong*，ZHAO Yue-chen，LUO Feng-jian，CHEN Zong-mao，CUI Xin-yi，ZHOU Li，LOU Zheng-yun |
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 |
|
| Hits: 2277 |
| Download times: 949 |
| Abstract: |
| 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. |
| Close |