饮用水中多氯联苯的全自动固相萃取-气相色谱/三重四级杆质谱测定法  

Determination of polychlorinated biphenyls in drinking water by automatic solid phase extraction-gas chromatography/quadrupole mass spectrometry

作　　者：姚铭栋 王余萍[1] 王冬梅[1] 

机构地区：[1]河南省安阳市疾病预防控制中心,455000

出　　处：《职业与健康》2015年第19期2634-2636,共3页Occupation and Health

摘　　要：目的建立一种同时测定饮用水中7种多氯联苯含量的全自动固相萃取-气相色谱/三重四极杆质谱（GC/MS/MS）方法。方法用盐酸调水样使p H值小于2,过C18萃取柱,乙酸乙酯、二氯甲烷洗脱,洗脱液在40℃水浴中氮吹近干,用正己烷定容,GC-MS/MS测定,内标法定量。结果 7种多氯联苯在27.9 min内分离,在5-500μg/L范围内相关系数r2均在0.994以上,0.005和0.05μg/L两个水平加标回收率在80%-110%之间,相对标准偏差均小于10%,检出限为0.01-0.05μg/L。结论该方法通过优化气相色谱条件,使7种多氯联苯得到较好的分离;选取丰度高的特征离子、最佳的碰撞能量,用GC-MS/MS检测特征离子的二级离子,减少了干扰,避免假阳性的出现,提高了灵敏度。该方法准确度和精密度高,适用于饮用水中7种多氯联苯痕量的检测和确证。[Objective]To establish a method for simultaneous determination of 7 polychlorinated biphenyls（ PCBs） in drinking water by automatic solid phase extraction-gas chromatography/quadrupole mass spectrometry（ GC/MS/MS）. [Methods]The water samples were treated by the hydrochloric acid to adjust the p H value（ less than 2）, and passed through a C18solid-phase extraction column, with the elution by ethyl acetate and methylenechloride. The eluent was treated by nitrogen blowing in water bath at 40 ℃ until it was nearly dry. Hexane was applied in constant volume, the extract was determined by GC-MS/MS, and the quantification was conducted by the internal standard method. [Results]7 kinds of PCBs were separated within 27.9 minutes. The calibration curves of 7 PCBs were linear（ correlation coefficient r20.994） within the range of 5-500 μg/L. The recoveries were between 80% and 110% at the addition mass concentration of 0.005 μg/L and 0.05 μg/L. The relative standard deviations were lower than 10%, and the limit of determination was 0.01-0.05 μg/L.[Conclusion]The method can effectively separate 7 PCBs by optimizing the gas chromatography conditions. Meanwhile, the method chooses the characteristic ion with high abundance and the best collision energy, and detects the secondary ion of characteristic ion by GC-MS/MS, as so to reduce the interference, avoid false positive, and improve the sensitivity. The method has high accuracy and precision, and it is suitable for the determination and confirmation of 7 PCBs in drinking water.

关 键 词：多氯联苯 气相色谱/三重四极杆质谱 固相萃取 饮用水 

分 类 号：R115[医药卫生—公共卫生与预防医学]