非衍生-离子色谱-三重四极杆质谱测定环境水样中有机磷

Determination of Organic Phosphines in Environmental Water by Non-derivatization-Ion Chromatography-Triple Quadrupole Mass Spectrometry

建立了一种非衍生-离子色谱-三重四极杆质谱法测定环境水样中有机磷(草甘膦、氨甲基膦酸、草铵膦、杀木膦和乙烯利)的方法。环境水样经RP-C18固相萃取柱和Ba柱除去杂质后,滤液无须衍生化,可直接进行定量分析。有机磷通过AS 19阴离子色谱柱分离,在负离子模式下以多反应监测方式(MRM)进行检测。结果表明,草甘膦、氨甲基膦酸和草铵膦在0.10~10.0μg/L范围内的线性相关系数(r)均>0.999,检出限分别为0.02,0.03和0.03μg/L,相对标准偏差(RSD)分别为2.8%~4.7%,5.4%~11.7%和5.1%~7.4%。杀木膦和乙烯利在0.02~2.00μg/L范围内的r值均>0.999,检出限分别为0.007和0.004μg/L,RSD分别为3.7%~5.8%和2.1%~13.2%。对实际水样进行测定,各目标物的加标回收率为70.0%~120%。该方法操作简便,精密度好,准确度高,适用于环境水样中5种极性有机磷的测定。

A method for the determination of glyphosate,aminomethyl phosphonic acid,glufosinate,fosamine ammonium and ethephon in environmental water by non-derivatization-ion chromatography-triple quadrupole mass spectrometry(IC-MS/MS)was established.The environmental water samples were filtered through RP-C18 solid phase extraction column and Ba column to remove impurities,and then the filtrate was directly subjected to quantitative analysis without derivatization.The organic phosphines were separated by AS 19 anion column and determined by triple quadrupole mass spectrometry in negative electrospray ion source mode under multiple reaction monitoring(MRM).Results showed that the correlation coefficients of glyphosate,aminomethyl phosphonic acid and glufosinate were all greater than 0.999 in the range of 0.10~10.0μg/L.The detection limits of glyphosate,aminomethyl phosphonic acid and glufosinate were 0.02,0.03 and 0.03μg/L,respectively.The relative standard deviations were 2.8%~4.7%,5.4%~11.7%and 5.1%~7.4%,respectively.The correlation coefficients of fosamine ammonium and ethephon were all greater than 0.999 in the range of 0.02~2.00μg/L.The detection limits of fosamine ammonium and ethephon were 0.007 and 0.004μg/L,respectively.The relative standard deviations were 3.7%~5.8%and 2.1%~13.2%,respectively.The sample recoveries of target compounds were in the range of 70.0%~120%.This method is suitable for the determination of five polar organic phosphines in environmental water samples with non-derivatization,simple operation,good repeatability and high accuracy.