水中23种半挥发性有机物三重四极杆气相色谱质谱联用测定法  

Determination of 23 kinds of semi-volatile organic compounds in water by gas chromatography-triple quadrupole mass spectrometry

作　　者：林华影[1] 李一丹[1] 张伟[1] 林瑶[1] 张琼[1] LIN Hua-ying;Ll Yi-dan;ZHANG Wei;LIN Yao;ZHANG Qiong(Laboratory Department of Fuzhou Disease Prevention and Control Center, Fuzhou Fujian, 350004, Chin)

机构地区：[1]福州市疾病预防控制中心检验科,福建福州350004

出　　处：《职业与健康》2017年第24期3344-3349,共6页Occupation and Health

摘　　要：目的建立一种测定水中23种半挥发性有机物的三重串联四极杆气相色谱质谱联用的分析方法。方法水样使用C18固相萃取小柱提取后,以二氯甲烷、乙酸乙酯和甲醇洗脱浓缩,DB-5MS毛细管柱分离,以三重串联四极杆气相色谱质谱联用多反应监测模式(MRM)进行测定,内标法定量。结果能简便有效地分析检测水中23种半挥发性有机物,各组份的相关系数大于0.998 1,方法的相对标准偏差小于3.42%,检出限为(0.010~0.037)μg/L,3个浓度水平的加标回收率为86.7%~106.9%。结论方法具有良好的选择性、灵敏度和准确度,化学背景低,对各种水样适应性好,用于水中23种半挥发性有机物的同时检测分析,结果令人满意。[Objective]To establish a method for the simultaneous determination of 23 kinds of semi-volatile organic compounds in water by gas chromatography coupled with triple quadrupole mass spectrometry.[Methods]Water sample was extracted on C18 solid phase column and eluted with dichloromethane,ethyl acetate methanol then separated by GC with a DB-5 MS capillary column. The extracts were analyzed by gas chromatography coupled with triple quadrupole mass spectrometry under multiple reaction monitoring（MRM） model,and the internal standard method was used for quantification.[Results]The method could effectively separate and determinate 23 kinds of semi-volatile organic compounds in water. The correlation coefficient was greater than 0.998 1,relative standard deviation was less than 3.42%,the limits of quantification were（0.010-0.037）μg/L,and the recoveries determined at three concentration levels were 86.7%-106.9%.[Conclusion]The method shows good selectivity,sensitivity and accuracy,and it has low chemical background and good adaptility to various water samples. The results of this method are satis-factory for simultaneous determination of 23 kinds of semi-volatile organic compounds in water.

关 键 词：水 半挥发性有机物 固相萃取 三重四极杆气相色谱质谱联用 

分 类 号：R115[医药卫生—公共卫生与预防医学]