饮用水中七类半挥发性有机物的气相色谱-三重四级杆串联质谱测定法

Determination of seven groups of semi-volatile organic compounds in drinking water by gas chromatography-triple quadruples mass spectrometry

目的建立饮用水中七类半挥发性有机物(SVOCs)的气相色谱-三重四级杆串联质谱-多反应监测方法(GC-MSMS-MRM)的测定方法。方法采集40 L末梢水经XAD-2、椰壳活性炭固相萃取柱双柱串联进行富集,XAD-2萃取柱用甲醇-丙酮(7∶3,V/V)、丙酮-正己烷(1∶1,V/V)、二氯甲烷依次洗脱,活性炭萃取柱用丙酮-正己烷(1∶1,V/V)、二氯甲烷洗脱,洗脱液自然挥干,复溶于1 ml甲醇,以GC-MS-MS-MRM定性定量测定。结果七类SVOCs在1~5000 ng/ml范围内,线性关系良好(R2>0.995),回收率多在70%~110%,RSD多低于20%,检出限为0.003~1.250 ng/L。末梢水中共检出37种SVOCs,包括7种我国水中优先控制SVOCs,16种美国EPA水中优先控制SVOCs;检出4种《生活饮用水标准》(GB5749—2006)规定的SVOCs,但均未超过浓度限值。该方法检测的末梢水中以邻苯二甲酸酯为主要检出SVOCs。结论该方法灵敏度高、特异性好、抗干扰能力强,适合于水中七类SVOCs的定性定量测定。

Objective To develop a method for detecting seven groups of semi-volatile organic compounds(SVOCs)in drinking water by gas chromatography-triple quadruples mass spectrometry with multiple reaction monitoring(GC-MS/MS-MRM).Methods Water samples(40 L)were extracted by XAD-2-activated carbon tandem solid-phase extraction(SPE)columns.XAD-2 column was eluted sequentially with methanol-acetone(7∶3,V/V),acetone-n-hexane(1∶1,V/V)and dichloromethane,activated carbon column was eluted sequentially with acetone-n-hexane(1∶1,V/V)and dichloromethane.The eluents were naturally air dried and dissolved in 1 ml methanol and analyzed qualitatively and quantitatively by GC-MS/MS-MRM.Results The regression equation of seven SVOCs showed a good linear relationship within 1-5000 ng/ml(R2>0.995).The recoveries of most SVOCs were 70%-110%,and the relative standard deviations were below 20%.The detection limits were 0.003-1.250 ng/L.A total of 37 kinds of SVOCs were detected in tap water,of which seven kinds were listed in China’s priority pollutants,16 kinds in US EPA’s priority pollutants,and four kinds in Standards for Drinking Water Quality(GB 5749-2006),but none exceeded the standards.Overall,phthalates were the dominant detectable contaminants in tap water.Conclusion This method is sensitive,selective,and anti-interfered,and suitable for detecting seven groups of SVOCs in drinking water qualitatively and quantitatively.