摘要
目的建立生活饮用水中10种乙醇胺类化合物的气相色谱-质谱联用测定方法。方法在1 L水样中加入1 mg硫代硫酸钠去除余氯,调节溶液pH=10,水样以5 mL/min的速度过MCX阳离子固相萃取小柱,5%甲醇淋洗杂质,抽干小柱,5%氨化甲醇15 mL洗脱剂洗脱,洗脱液经无水硫酸钠脱水,水浴温度50℃,氮气吹至近干,甲醇定容至1.0 mL,经CP-Sil 8 CB色谱柱分离后,气相色谱-质谱法测定,外标法定量,检测水中10种乙醇胺类化合物。结果在优化的实验条件下,10种醇胺类化合物在5~100μg/mL浓度范围内线性关系良好,线性系数r>0.9991,方法检出限为1.2~2.8μg/mL,平均回收率在70.7%~84.9%,相对标准差(RSD)在4.8%~11.1%。结论该方法简便、重现性好,适用于水中10种乙醇胺类化合物的同时测定。
Objective To develop a gas chromatography-mass spectrometry for simultaneous determination of 10 types of ethanol-amine compounds in drinking water.Methods Water samples(1 L)were added with 1 mg sodium thiosulfate to remove residual chlorine and the solution pH was adjusted to 10.Water samples were separated on MCX solid-phase extraction columns at a speed of 5 mL/min,and the impurities were eluted with 5%methanol.The column was dried and eluted with 15 mL of 5%amonium methanol.The elution solution was dehydrated in anhydrous sodium sulfate,placed in water bath at 50 C,dried in nitrogen and adjusted to 1.0 mL with methanol.Following separation on CP-Sil 8 CB chromatographic columns,the 10 types of ethanolamine compounds were determined in drinking water using gas chromatography-mass spectrometry and a quantitative analysis was conducted with the external standard method.Results Under optimized experimental conditions,gas chromatography-mass spectrometry showed a good linear relationship for determination of 10 types of ethanolamine compounds at mass concentrations of 5 to 100μg/mL(r>0.9991),and the assay showed a limit of detection of 1.2 to 2.8μg/mL,mean recovery of 70.7%to 84.9%and relative standard deviations of 4.8%to 11.1%.Conclusions The developed gas chromatography-mass spectrometry is simple and highly reproducible,which is suitable for simultaneous determination of 10 types of ethanolamine compounds in drinking water.
作者
刘波
霍宗利
张婧婧
LIU Bo;HUO Zong-li;ZHANG Jing-jing(Taizhou Municipal Center for Disease Control and Prevention,Taizhou,Jiangsu 225300,China;不详)
出处
《江苏预防医学》
CAS
2023年第5期524-527,共4页
Jiangsu Journal of Preventive Medicine
基金
江苏省333高层次人才培养工程([2022]3-7-023)。
关键词
乙醇胺类化合物
生活饮用水
气相色谱-质谱法
Ethanolamine compounds
Drinking water
Gas chromatography-mass spectrometry
