超高效合相色谱-四极杆飞行时间质谱法测定水果和茶叶中手性农药顺式-氟环唑对映体残留  

Residue Determination of cis-Epoxiconazole Enantiomers in Fruit and Tea by Ultra Performance Convergence Chromatography Combined with Quadrupole Time-of-Flight Mass Spectrometry

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

机构地区：[1]天津农学院园艺园林学院,天津300384 [2]中国农业科学院茶叶研究所农产品质量安全研究中心,杭州310008

出　　处：《分析化学》2016年第8期1200-1208,共9页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学青年基金(No.21107137);国家茶叶产业技术体系(No.CARS-23);浙江省自然科学基金(No.Y3100259);中国农业科学院创新工程资助~~

摘　　要：利用超高效合相色谱-四极杆飞行时间质谱(UPC^2-QTOF/MS),建立了顺式-氟环唑在苹果、葡萄和茶叶中的手性对映体拆分与残留分析方法。对合相色谱条件(流动相改性剂及比例、色谱柱温度、背压、辅助溶剂等)进行了优化。样品采用乙腈提取,Cleanert TPT或Pesti-Carb柱净化,Chromega Chrial CCA柱进行分离,以CO_2/异丙醇(95∶5,V/V)为流动相,流速2.0 m L/min,动态背压13.79 MPa,柱温30℃,离子化辅助溶剂为2 mmol/L甲酸铵的甲醇-水(1∶1,V/V),采用超高效合相色谱-四极杆飞行时间质谱分析测定,基质外标法定量。结果表明,本方法的线性范围为0.01 mg/L^1.00 mg/L,相关系数大于0.99;在0.005,0.025和0.25 mg/kg添加浓度水平下,苹果和葡萄中顺式-氟环唑手性对映体平均回收率(n=6)为67.9%~92.8%,相对标准偏差小于10%,方法定量限为0.005 mg/kg;在0.01,0.05和0.5 mg/kg添加浓度水平下,茶叶中顺式-氟环唑手性对映体平均回收率(n=6)为74.1%~84.0%,相对标准偏差小于8%,方法定量限为0.01 mg/kg。本方法准确、简便、可靠,可以满足残留分析的要求。Abstract A chiral separation and residue determination method for cis-epoxiconazole enantiomers in apple, grape and tea samples was developed and validated by ultra performance convergence chromatography combined with quadrupole time-of-flight mass spectrometry （ UPC2-QTOF/MS） . The Chrial CCA column was used to separate cis-epoxiconazole enantiomers and the chromatography conditions （ mobile phase modifier and proportion, column temperature, automated backpressure regulator, and auxiliary solvent ） were optimized. Samples were extracted by acetonitrile, and respectively purified by Cleanert TPT or Pesti-Carb solid phase extraction （ SPE ） columns, then analyzed by UPC2-QTOF/MS. The optimum conditions were as follows：mobile phase was CO2/isopropanol （95： 5, V/V）, flow-rate was 2. 0 mL/min, automated backpressure regulator （ABPR） was 13. 79 MPa, column temperature was 30℃, with a post-column mauxiliary solvent of methanol/water （1：1, V/V） containing 2 mmol/L ammonium formate. The analyte was quantified by matrix external standard method. The results showed that linear range of this method was 0. 01-1. 00 mg/L, and the correlation coefficients were above 0 . 99 . The recoveries of cis-epoxiconazole enantiomers at three spiked levels （0. 005, 0. 025 and 0. 25 mg/kg） in fruit matrix were 67. 9%-92. 8% with relative standard deviations （RSDs, n=6） less than 10%, and the limit of quantification （LOQ） of enantiomers was 0. 005 mg/kg. The recoveries of cis-epoxiconazole enantiomers at three spiked levels （0. 01, 0. 05 and 0. 5 mg/kg） in black tea were 74 . 1% -84 . 0% with RSDs （ n=6 ） less than 8%, and the LOQ for these two enantiomers was 0. 01 mg/kg. This method is rapid, convenient and reliable, and could meet the requirement of residue analysis.

关 键 词：手性对映体 残留分析 顺式-氟环唑 葡萄 苹果 茶叶 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] TS207.53[理学—化学]