摘要
采用QuEChERS方法净化,建立了GC/ECD法同时检测茶叶和土壤中噻虫嗪、虫螨腈和高效氯氟氰菊酯残留的分析方法。样品经水浸润后,乙腈提取,适量PSA、GCB和Florisil混合填料净化提取液,GC/ECD检测。噻虫嗪、虫螨腈和高效氯氟氰菊酯的响应分别在0.50~400、0.20~100、0.40~200μg/L质量浓度范围内线性良好,相关系数r均大于0.99,检出限分别为0.25、0.05、0.10μg/L。茶叶和土壤样品中,噻虫嗪、虫螨腈和高效氯氟氰菊酯的平均加标回收率为62%~108%,相对标准偏差(RSDs)不大于15.8%,方法的定量下限(LOQs)均不大于10μg/kg。方法简便、快速,能够满足茶叶和土壤中上述3种不同极性农药残留同时检测的需要。采用该方法测定了3种农药在茶园茶叶和土壤中的残留量,结果满意。
A GC/ECD method for the simultaneous analysis of thiamethoxam, chlorfenapyr and lambda-cyhalothrin residues in tea and soil was developed and validated. The samples were extracted with acetonitrile after water soaking, and purified by QuEChERS method using PSA, GCB and Flori- sil as adsorbents, then determined by GC/ECD. The result showed that the calibration curves were lin- ear in the ranges of 0. 50 -400~μg/L for thiamethoxam, 0. 20 - 100μg/L for chlorfenapyr and 0. 40 - 200 μg/L for lambda-cyhalothrin, with correlation coefficients more than 0. 99. The limits of detection (LODs) for thiamethoxam, chlorfenapy and lambda-cyhalothrin were 0. 25, 0. 05, 0. 10 μg/L, re- spectively. The average recoveries in tea and soil at three spiked levels were between 62% and 108% with RSDs( n = 5 )no more than 15.8% , and the limits of quantitation(LOQs) were lower than 10 μg/ kg. This method is easy, quick, effective and safe, and can meet the requirements for simultaneous residue determination of thiamethoxam, chlorfenapyr and lambda-cyhalothrin in tea and soil samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第4期393-400,共8页
Journal of Instrumental Analysis
基金
国家自然科学青年基金(21107137)
国家茶叶产业技术体系(CARS-23)
农业部农药残留登记试验项目(2010P533)