超声萃取高效液相色谱法测定土壤中乙草胺的残留量
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摘要
建立了一种从土壤中超声提取乙草胺并采用高效液相色谱法测定其残留量的分析方法.选用正己烷∶丙酮(配比为4∶1)为萃取剂,超声振荡萃取时间为20min,使用BDS Hypersil C18(4.6mm×250mm,5μm)色谱柱,以乙腈∶水=70∶30为流动相,流速为1mL·min-1,紫外检测波长为210nm.测定结果显示:乙草胺的保留时间为4.875min,线性相关系数为0.998 4;相对标准偏差(RSD)为3.5%;在四个梯度质量浓度水平上,平均回收率是97.09%,该分析方法的检出限为0.18ng·mL-1,该方法简单快捷,灵敏度高,准确性好,可作为乙草胺的检测方法.
A method was introduced for ultrasonic extraction and measurement of acetochlor residue by high efficiency liquid chromatography.Operation process:n-hexane and acetone(ratio of 4∶1)was used as extraction,for 20 min.A BDS Hypersil C18 column(4.6 mm×250 mm,5μm)was used with a mobile phase of acetonitrile and water(70∶30,V/V).Under the condition of the flow rate of 1 mL·min-1 and UV detection wavelength of 210 nm,the retention time of acetochlor was 4.875 min;the linear correlation coefficient was 0.9984;the relative standard deviation(RSD)was 3.5;at the four gradient mass concentration levels,the average recovery was 97.05 and the measurement limit was 0.18 ng·mL-1.The method was simple,quick,sensitive and accurate,which can be used for the measurement of acetochlor.
A method was introduced for ultrasonic extraction and measurement of acetochlor residue by high efficiency liquid chromatography.Operation process:n-hexane and acetone(ratio of 4∶1)was used as extraction,for 20 min.A BDS Hypersil C18 column(4.6 mm×250 mm,5μm)was used with a mobile phase of acetonitrile and water(70∶30,V/V).Under the condition of the flow rate of 1 mL·min-1 and UV detection wavelength of 210 nm,the retention time of acetochlor was 4.875 min;the linear correlation coefficient was 0.9984;the relative standard deviation(RSD)was 3.5;at the four gradient mass concentration levels,the average recovery was 97.05 and the measurement limit was 0.18 ng·mL-1.The method was simple,quick,sensitive and accurate,which can be used for the measurement of acetochlor.
引文
[1]王姗姗,王颜红,王万红,等.阿拉特津和乙草胺在玉米和土壤中残留动态研究[J].土壤通报,2011,42(5):1231-1232.
[2]金党琴,龚爱琴,丁邦东,等.快速溶剂萃取高效液相色谱法测定土壤中乙草胺和烯草酮残留[J].安徽农业大学学报,2018,45(2):1-4.
[3]黄碧燕,韦宇宁,李小夏,等.气相色谱法同时测定土壤中毒死稗、乙草胺和丁草胺残留量[J].广西科学院学报,2010,26(3):255-257.
[4]李瑞娟,张晓梅,于建垒,等.气相色谱法同时测定玉米和土壤中乙草胺和2,4-滴丁酯残留[J].现代农药,2011,10(2):34-36.
[5]刘晓明,郭平毅,冯翠萍,等.高效液相色谱法检测玉米及玉米叶中乙草胺的残留量[J].山西农业大学学报(自然科学版),2012,32(1):5-8.
[6]苏旺苍,吴仁海,王恒亮,等.甲酷化植物油基烟嘧磺隆·乙草胺混配制剂高效液相色谱分析[J].杂草科学,2013,3(31):48-50.
[7]梅文泉,黎其万,方海仙,等.QuEChERS-气相色谱-质谱法测定土壤中6种酰胺类除草剂残留[J].色谱,2017,35(12):1317-1321.
[8]栾燕,汤先伟,张玉黔,等.环境样品中乙草胺和莠去津的气相色谱-质谱测定法[J].环境与健康杂志,2005,25(4):294-295.
[9]王铁龙,胡继业.土壤和水体中20种除草剂的气相色谱-质谱法多残留分析[J].农药学学报,2012,14(6):629-634.
[10]闫蕊,邵明媛,鞠福龙,等.加速溶剂萃取-高效液相色谱串联质谱法测定土壤中农药残留[J].分析化学,2013,41(2):315-316.
[11]李菊颖,郭欣妍,何健,等.玉米粉中吡虫啉、三唑酮、乙草胺与异丙甲草胺QuEChERS/高效液相色谱-串联质谱快速检测[J].分析测试学报,2017,36(6):783-787.
[2]金党琴,龚爱琴,丁邦东,等.快速溶剂萃取高效液相色谱法测定土壤中乙草胺和烯草酮残留[J].安徽农业大学学报,2018,45(2):1-4.
[3]黄碧燕,韦宇宁,李小夏,等.气相色谱法同时测定土壤中毒死稗、乙草胺和丁草胺残留量[J].广西科学院学报,2010,26(3):255-257.
[4]李瑞娟,张晓梅,于建垒,等.气相色谱法同时测定玉米和土壤中乙草胺和2,4-滴丁酯残留[J].现代农药,2011,10(2):34-36.
[5]刘晓明,郭平毅,冯翠萍,等.高效液相色谱法检测玉米及玉米叶中乙草胺的残留量[J].山西农业大学学报(自然科学版),2012,32(1):5-8.
[6]苏旺苍,吴仁海,王恒亮,等.甲酷化植物油基烟嘧磺隆·乙草胺混配制剂高效液相色谱分析[J].杂草科学,2013,3(31):48-50.
[7]梅文泉,黎其万,方海仙,等.QuEChERS-气相色谱-质谱法测定土壤中6种酰胺类除草剂残留[J].色谱,2017,35(12):1317-1321.
[8]栾燕,汤先伟,张玉黔,等.环境样品中乙草胺和莠去津的气相色谱-质谱测定法[J].环境与健康杂志,2005,25(4):294-295.
[9]王铁龙,胡继业.土壤和水体中20种除草剂的气相色谱-质谱法多残留分析[J].农药学学报,2012,14(6):629-634.
[10]闫蕊,邵明媛,鞠福龙,等.加速溶剂萃取-高效液相色谱串联质谱法测定土壤中农药残留[J].分析化学,2013,41(2):315-316.
[11]李菊颖,郭欣妍,何健,等.玉米粉中吡虫啉、三唑酮、乙草胺与异丙甲草胺QuEChERS/高效液相色谱-串联质谱快速检测[J].分析测试学报,2017,36(6):783-787.