HPLC-MS/MS法分析30%硝磺·烟·莠可分散油悬浮剂含量
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摘要
目的:采用HPLC-MS/MS建立30%硝磺草酮·烟嘧磺隆·莠去津可分散油悬含量检测方法。方法:采用高效液相色谱-串联质谱法,以60%水(0.1%甲酸水)溶液+40%乙腈为流动相,使用以Agilent Eclipse Plus C18 1.8μm填料的不锈钢柱和MSD检测器,对试样中的硝磺草酮、烟嘧磺隆和莠去津进行测定,外标法定量。结果:该方法的硝磺草酮、烟嘧磺隆和莠去津线性相关系数分别为0.9993、0.9996和0.9999,变异系数分别为0.82%、0.46%和0.40%,平均回收率分别为102.85%、106.23%和104.86%。结论:该方法克服以往用液相色谱法高检出限,保留时间长等缺陷,而本方法运行时间短,操作简单,分离效果佳,准确度和精密度高,可用于30%硝磺·烟嘧·莠可分散油悬浮剂含量检测。
In this study,we established a method to detect the content of Mesotrione-Nicosulfuron-Atrazine 30% OF by HPLC-MS/MS.The separation and quantitative analysis of Mesotrione,Nicosulfuron and Atrazine samples were conducted by HPLC-MS/MS and MSD detector with the mixture of water(with 0.1 % formic) and acetonitrile(60∶40,by volume) as mobile phase,and with Agilent Eclipse Plus C18 1.8 μm column as fixed phase.The results showed that the linear correlation coefficients of Nicosulfuron,Nicosulfuron and Atrazine were 0.9993,0.9996 and 0.9999,the variation coefficients were 0.82%,0.46% and 0.40%,the average recovery rates were 102.85%、106.23% and 104.86%,respectively.This method has overcome defects such as high detection limit and long retention time by liquid chromatography,and is simple to operate;the accuracy,precision and sensitivity are all satisfactory,which is suitable for the analysis of Mesotrione-Nicosulfuron-Atrazine 30% OF.
In this study,we established a method to detect the content of Mesotrione-Nicosulfuron-Atrazine 30% OF by HPLC-MS/MS.The separation and quantitative analysis of Mesotrione,Nicosulfuron and Atrazine samples were conducted by HPLC-MS/MS and MSD detector with the mixture of water(with 0.1 % formic) and acetonitrile(60∶40,by volume) as mobile phase,and with Agilent Eclipse Plus C18 1.8 μm column as fixed phase.The results showed that the linear correlation coefficients of Nicosulfuron,Nicosulfuron and Atrazine were 0.9993,0.9996 and 0.9999,the variation coefficients were 0.82%,0.46% and 0.40%,the average recovery rates were 102.85%、106.23% and 104.86%,respectively.This method has overcome defects such as high detection limit and long retention time by liquid chromatography,and is simple to operate;the accuracy,precision and sensitivity are all satisfactory,which is suitable for the analysis of Mesotrione-Nicosulfuron-Atrazine 30% OF.
引文
[1]胡玫,过欣雨.24%硝磺·烟嘧·莠可分散油悬浮剂高效液相色谱分析[J].河南化工,2017(2):54-56.
[2]吴艳芳,徐家俊,孟令涛,等.26%硝磺草酮·烟·莠油悬剂高效液相色谱分析[J].农药,2014,53(1):26-27.
[3]姚菊仙,杨丽凰,李榆庆.28%烟·硝·莠去津可分散油悬浮剂的分析方法[J].云南化工,2018,45(6):105-107.
[2]吴艳芳,徐家俊,孟令涛,等.26%硝磺草酮·烟·莠油悬剂高效液相色谱分析[J].农药,2014,53(1):26-27.
[3]姚菊仙,杨丽凰,李榆庆.28%烟·硝·莠去津可分散油悬浮剂的分析方法[J].云南化工,2018,45(6):105-107.