固相萃取富集-气相色谱法测定地表水中5种三唑类杀菌剂
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摘要
目的:研究一种利用固相萃取装置净化、富集地表水样品中的5种三唑类杀虫剂(三唑醇、三唑酮、戊唑醇、三唑磷、腈菌唑),GC-ECD法检测的分析方法。方法:地表水样品经固相萃取柱富集待测化合物,甲醇洗脱,洗脱液上气相色谱仪检测,外标法计算5种三唑类杀虫剂的残留量。结果方法的加标回收率范围在85.3～107.2%之间;线性范围在0.05～10.0μg/mL范围内,线性系数R~2均大于0.995;检出限在0.002～0.005μg/mL之间;重复性和精密度相对标准偏差(n=6)均不高于5.0%。结论:研究结果表明,方法具有线性范围广、前处理操作简单、灵敏度高等优点,适用于地表水样品中该5种三唑类杀菌剂的检测。
The residual amount of 5 triazole fungicides(triadimenol,triazolone,tebuconazole,triazolphos,myclobutanil)were eluted with methanol and determined by external standard method.The recovery was 85.3%-107.2%,the linear range was 0.05-10.0μg/mL,the correlation coefficients R~2 was more than 0.995,and the detection limit was 0.002-0.005μg/mL.The relative standard deviation(RSD)(n=6)of repeatability and precision were no more than 5.0%.This method has the advantages of wide linear range,simple pre-treatment and high sensitivity,is suitable for the detection of the 5 triazole fungicides in surface water samples.
The residual amount of 5 triazole fungicides(triadimenol,triazolone,tebuconazole,triazolphos,myclobutanil)were eluted with methanol and determined by external standard method.The recovery was 85.3%-107.2%,the linear range was 0.05-10.0μg/mL,the correlation coefficients R~2 was more than 0.995,and the detection limit was 0.002-0.005μg/mL.The relative standard deviation(RSD)(n=6)of repeatability and precision were no more than 5.0%.This method has the advantages of wide linear range,simple pre-treatment and high sensitivity,is suitable for the detection of the 5 triazole fungicides in surface water samples.
引文
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[5]郭亚芸,史红梅,韩晓梅,等.浸入式固相微萃取-气相色谱-质谱联用法分析葡萄酒中三唑类农药[J].分析试验室,2017,28(5):811-814.
[7]庄乾坤,郑和辉,卞战强,等.超高效液相色谱-串联质谱法测定饮用水中6种三唑类杀菌剂[J].中国卫生检验杂志,2016,26(2):153-155.
[8]赵春娟,高文惠.高效液相色谱法检测饲料中三唑类杀菌剂残留[J].中国饲料,2015,32(3):24-25.
[9]吴小春,姚科伟,魏双利,等.快速溶剂萃取-气相色谱质谱法测定土壤中戊唑醇残留量[J].化学分析计量,2015,24(3):76-78.
[10]高文惠,王姣姣.分子印迹固相萃取膜-高效液相色谱法检测粮谷中的三唑类杀菌剂[J].现代食品科技,2014,30(12):225-229.
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[12]郭亚芸,丁燕,韩晓梅,等.超声辅助-分散液液微萃取-气相色谱/质谱法测定葡萄酒中三唑类农药残留[J].分析科学学报,2018,26(3):409-412.