摘要
建立生活饮用水中二氯乙酸、三氯乙酸2种卤代酸残留量的气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测方法,比较硫酸-甲醇溶液、三甲基硅重氮甲烷(trimethylsilyl diazomethane,TMSCHN_2)己烷溶液衍生化试剂用于2种卤代酸化合物衍生化反应的差异。生活饮用水样品经甲基叔丁基醚超声提取,弗罗里硅土固相萃取柱(Florisil)净化,硫酸-甲醇溶液、三甲基硅重氮甲烷己烷溶液衍生,采用GC-MS/MS多反应监测模式分析,外标法定量。结果表明,采用优化后条件,二氯乙酸、三氯乙酸在0.005 mg/L～0.200 mg/L的定量范围内,线性关系良好,相关系数均在0.99以上。选取3种不同水样品,在空白样品添加浓度为0.02、0.04、0.1 mg/L的范围内,二氯乙酸、三氯乙酸的平均回收率范围为86.1%～96.5%,相对标准偏差小于5.2%。二氯乙酸、三氯乙酸经TMSCHN_2衍生后的响应是经硫酸-甲醇溶液衍生后响应的1.69、1.71倍。采用TMS-CHN_2衍生的方法,大大缩短了检测时间,提高检测效率,降低了检测成本,有利于大批水样品的日常检测。
A gas chromatography-tandem mass spectrometry(GC-MS/MS)was established for the determination of dichloracetic acid and trichloroacetic acid residues in drinking water.The differences in the derivatization reaction of dichloracetic acid and trichloroacetic acid by sulfuric acid-methanol solution and trimethylsilyl diazomethane(TMS-CHN2)hexane solution were compared.Sulfuric acid-methanol solution and TMS-CHN2 hexane solution were used as the derivatization reagents for dichloracetic acid and trichloroacetic acid are reported in this paper.Samples of drinking water were extracted with methyl tert-butyl ether and then derived by sulfuric acid-methanol solution and TMS-CHN2 hexane solution.A cleanup step using Florisil SPE cartridge was applied,and then quantified by external standard method in multiple reactions monitoring mode(MRM).Under the optimized conditions,the target concentrations and peak areas were linearly correlated in the range of 0.005 mg/L-0.200 mg/L,and the correlation coefficients are greater than 0.99.Recovery studies were carried out on spiked matrices(three different water samples)with dichloracetic acid and trichloroacetic acid at spiking levels of 0.02,0.04,0.1 mg/L.The mean recoveries were 86.1%-96.5%,with relative standard deviations less than 5.2%.The response for the derivatives of dichloracetic acid and trichloroacetic acid by the TMS-CHN2 hexane solution in water was 1.69,1.71 times of dichloracetic acid and trichloroacetic acid by the sulfuric acid-methanol solution.The method of TMS-CHN2 hexane solution derivation was adopted,which greatly reduces the detection time,improves the detection efficiency,reduces the detection cost,and is conducive to the daily detection of a large number of water samples.
作者
胡松
陈卢涛
周婷婷
俞璐萍
黎斌
刘小羽
胡晋峰
朱萌萌
HU Song;CHEN Lu-tao;ZHOU Ting-ting;YU Lu-ping;LI Bin;LIU Xiao-yu;HU Jin-feng;ZHU Meng-meng(Greentown Agricultural Detection Technology Co.,Ltd.,Hangzhou 310000,Zhejiang,China;State Key Laboratory of Tea Plant Biology and Utilization,College of Tea and Food Science&Technology,Anhui Agricultural University,Hefei 230036,Anhui,China)
出处
《食品研究与开发》
CAS
北大核心
2018年第22期101-106,共6页
Food Research and Development
关键词
二氯乙酸
三氯乙酸
硫酸-甲醇
三甲基硅重氮甲烷
气相色谱-串联质谱法
dichloracetic acid
trichloroacetic acid
sulfuric acid-methanol solution
trimethylsilyl diazomethane hexane solution
gas chromatography-tandem mass spectrometry
