气相色谱-串联质谱法同时测定水中28种溴代阻燃剂  

Simultaneous determination of 28 brominated flame retardants in water using gas chromatography-tandem mass spectrometry

作　　者：李琰[1] 郝春慧 董洁 崔伟 陆修双 李强[2] LI Yan;HAO Chun-hui;DONG Jie;CUI Wei;LU Xiu-shuang;LI Qiang(Physical and Chemical Department,Minhang District Center for Disease Control and Prerention,Shanghai 201101,China;不详)

机构地区：[1]上海市闵行区疾病预防控制中心理化检验科,上海201101 [2]上海市普陀区疾病预防控制中心理化检验科

出　　处：《中国卫生检验杂志》2022年第24期2972-2978,共7页Chinese Journal of Health Laboratory Technology

摘　　要：目的 建立水中28种溴代阻燃剂的气相色谱-串联质谱同时测定的方法。方法 取100 ml水样,加盐溶解后再加入同位素内标,用20 ml正己烷-甲基叔丁基醚(3:1,V/V)液液萃取2次,复合硅胶固相萃取柱净化,5 ml正己烷-二氯甲烷(1:1,V/V)洗脱3次,浓缩至近干后用100μl正己烷复溶,采用气相色谱-三重四级杆质谱法测定,多反应监测模式检测,内标法定量。结果 28种物质分离效果好,在2 ng/L~100 ng/L[其中十溴联苯醚和四溴邻苯二甲酸双(2-乙基己基)酯为20 ng/L~1 000 ng/L]内线性良好,相关系数为0.997 5~0.999 9;方法检出限为0.22 ng/L~6.58 ng/L;平均回收率为63.6%~128%;相对标准偏差为1.13%~23.0%。结论 该方法具有灵敏度高、精密度好、准确度高、通量高、分析周期短的优点,可以实现水中28种溴代阻燃剂的同时测定。Objective This study aims to establish a method for the simultaneous determination of 28 brominated flame retardants in water by gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods A total of 100 ml water sample was dissolved with salt and then added with isotope internal standard. The sample was extracted with 20 ml n-hexane-methyl tertiary butyl ether(3:1, V/V) for twice, purified by composite silica gel solid phase extraction column, eluted three times with 5 ml n-hexane-dichloromethane(1:1, V/V), concentrated to nearly dry, and then redissolved with 100 μl n-hexane and then analyzed by gas chromatography tandem mass spectrometry using multi-reaction monitoring mode and quantified by internal standard method. Results The separation effect of 28 substances was good, and the linearity was good in the range of 2 ng/L-100 ng/L [in which decabromobiphenyl ether and bis(2-ethylhexyl) tetrabromophthalate were within 20 ng/L-1 000 ng/L], and the correlation coefficient(r) was within 0.997 5-0.999 9. The detection limits of the method were within 0.22 ng/L-6.58 ng/L, the recoveries were within 63.6%-128% and the relative standard deviations(RSDs) were within 1.13%-23.0%. Conclusion This method has the advantages of high sensitivity, good precision, high accuracy, high flux and short analysis cycle. It can be used for the determination of various brominated flame retardants in water simultaneously.

关 键 词：溴代阻燃剂 气相色谱-串联质谱法 水 

分 类 号：O657[理学—分析化学]