利用优化后的QuEChERS前处理条件结合超高效液相色谱,建立果蔬中氰氟草酯和氰氟草酸残留的检测方法。样品采用V(乙腈)∶V(甲酸)=99∶1超声提取,随后用NaCl、无水MgSO4盐析分层,经乙二胺-N-丙基硅烷化硅胶(propylethylene diamine, PSA)、石墨化炭黑(graphitized carbon black, GCB)和无水MgSO4吸附剂组合净化,采用C18色谱柱分离,以甲醇-水-乙腈-0.1%磷酸为流动相,梯度洗脱,在248 nm下检测,以基质匹配标准溶液法定量。结果表明,氰氟草酯和氰氟草酸在0.01~10 μg/mL范围内线性关系良好,相关系数均大于0.998 9。氰氟草酯和氰氟草酸在7种果蔬基质中的平均加标回收率为73.1%~105.6%,相对标准偏差为1.5%~7.8%。方法检出限为1.0~2.5 μg/kg,定量限为10~20 μg/kg。该方法灵敏度高、重现性好,适用于果蔬中氰氟草酯和氰氟草酸残留的快速筛查和定量分析。
This study applied an optimized QuEChERS extraction technique coupled with ultra-high performance liquid chromatography (UPLC) to develop a method for the determination of cyhalofop-butyl and cyhalofop-caid residues in fruits and vegetables. The sample was extracted by sonication using a solution of acetonitrile-formic acid (99∶1, volume ratio), and then the extract was salted out with a mixture of anhydrous magnesium sulfate and sodium chloride, and purified by a combination of propylethylene diamine (PSA), graphitized carbon black (GCB), and anhydrous MgSO4 adsorbent, separated on a C18 column by gradient elution using a mobile phase consisting of methanol, water, acetonitrile, and 0.1% phosphate acid, and detected at a wavelength of 248 nm. The analytes were quantified by using matrix-matched standard solutions. Results showed that cyhalofop-butyl and cyhalofop-caid presented a good linear relationship between 0.01 and 10 μg/mL, with r (correlation coefficient) values > 0.998 9. The average spiked recoveries of cyhalofop-butyl and cyhalofop-caid in seven fruit and vegetable substrates were 73.1%-105.6% with a relative standard deviation (RSDs) of 1.5%-7.8%. The limits of detection and quantification ranged from 1 to 2.5 μg/kg and 10 to 20 μg/kg. This method described was of high sensitivity and good repeatability, which demonstrated that it was suitable for the rapid screening and quantitative analysis of cyhalofop-butyl and cyhalofop-caid residues in fruits and vegetables.
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