离子色谱-串联质谱法测定4类水质中7种极性有机磷

Determination of 7 Organic Phosphines in 4 Kinds of Water Qualities by Ion Chromatography-Tandem Mass Spectrometry

应用离子色谱-串联质谱法(IC-MS/MS)同时测定了地下水、地表水、生活污水和工业废水等4类水质中的草甘膦、草铵膦、氨甲基膦酸、杀木膦、乙烯利、双甘膦和增甘膦。这7种有机磷极性和水溶性强,用常规气相或液相的方法需要经衍生化后才能测定,且要严格控制前处理条件。该法水样用微孔滤膜和离子净化柱过滤后直接进样,经Ion Pac AS11-HC离子色谱柱分离、大气压电喷雾串联四极杆质谱仪负离子和正离子多反应监测模式检测(MRM)、外标法定量,结果表明,草甘膦、草铵膦、氨甲基膦酸、杀木膦、乙烯利、双甘膦和增甘膦分别在0.05~5.00、0.50~50.0、1.00~100.0、0.50~50.0、0.50~50.0、0.05~5.00、1.00~100.0μg/L范围内线性良好,线性相关系数均大于0.999;检出限0.007~0.40μg/L,相对标准偏差3.0%~20.0%,4类水样中7种有机磷的加标回收率范围86.9%~121.2%。该方法适用于水质中7种极性痕量有机磷的同时测定,无需繁琐的衍生化前处理过程,灵敏度高,操作简单,抗干扰性强。

Ion chromatography-tandem mass spectrometry(IC-MS/MS)was used to determine glyphosate(GLY),glufosinate(GLUF),aminomethyl phosphonic acid(AMPA),fosamine ammonium(FOAM),ethephon(ETH),N-Phosphonomethylaminodiacetic acid(PMIDA)and glyphosine(GLYP)in 4 kinds of water samples(groundwater,surface water,sewage and industrial wastewater).Polarity and solubility of 7 kinds organic phosphines are strong,with gas or liquid chromatography method need to determine after derivatization,and need to strictly control the pretreatment conditions.In this method,water samples were detected directly after filtration by microporous membrane and ion purification column.Ion Pac AS11-HC ion chromatographic column was selected for separation,atmospheric pressure anion and cation electrospray tandem quadrupole mass spectrometer multiple reaction monitoring mode(MRM)was selected for detection,external standard method was selected for quantification.The results showed that the 7 organic phosphines had the good linearity in the ranges of 0.05-5.00,0.50-50.0,1.00-100.0,0.50-50.0,0.50-50.0,0.05-5.00,1.00-100.0μg/L,respectively.The linear correlation coefficients were all greater than 0.999.The limits of detection were 0.007-0.40μg/L,the relative standard deviations(RSDs)were 3.0%-20.0%,and the recoveries of 7 kinds organic phosphines in 4 kinds of water samples were 86.9%-121.2%.The results showed that this method is suitable for the simultaneous determination of 7 polar trace organic phosphines in water.It has high sensitivity,simple operation and strong anti-interference,and does not need the complicated pre-treatment of derivatization.