摘要
目的建立工作场所空气中硫酸二甲酯(DMS)的柱前衍生-高效液相色谱测定方法。方法采用巯基吡啶浸渍硅胶管采集工作场所空气中DMS。DMS与巯基吡啶的衍生产物经流动相(流动相A为去离子水,流动相B为乙腈,体积比40∶60)洗脱,C18色谱柱分离,二极管阵列检测器检测,标准曲线法定量。结果DMS在质量浓度为0.17~40.00 mg/L时线性关系良好,相关系数为0.99995;检出限为0.05 mg/L,定量下限为0.17 mg/L,最低检出浓度和最低定量浓度分别为0.02和0.04 mg/m^(3)(均以采集4.5 L空气,解吸液体积为1.0 mL计算);平均解吸效率为98.40%~102.00%;批内、批间相对标准偏差分别为0.61%~3.92%和1.71%~6.00%。样品在常温下可以保存至少14 d。结论该方法适用于工作场所空气中DMS的检测。
Objective To establish a pre-column derivatization-high performance liquid chromatography method for detecting dimethyl sulfate(DMS)in workplace air.Methods DMS in workplace air was collected with mercaptopyridine impregnated silicone tube.The derivative of DMS and mercaptopyridine was eluted by mobile phase(phase A:water,phase B:acetonitrile,the volume ratio was 40∶60),and separated with a C18 column,then detected with diode array detector and quantitated by a standard curve.Results The linear range of DMS was 0.17-40.00 mg/L,with the correlation coefficient of 0.99995.The detection limit and the lower limit of quantitation were 0.05 and 0.17 mg/L respectively.The minimum detection concentration and minimum quantitation concentration were 0.02 and 0.04 mg/m^(3),respectively(air sample volume of 4.5 L,1.0 mL sample solution).The average desorption efficiency was 98.40%-102.00%.The within-run and between-run relative standard deviations were 0.61%-3.92%and 1.71%-6.00%,respectively.The samples could be stored at room temperature for at least 14 days.Conclusion This method can be used to detect DMS in workplace air.
作者
袁静
戎伟丰
胡嘉雯
何嘉恒
蒙瑞波
吴川
吴邦华
YUAN Jing;RONG Wei-feng;HU Jia-wen;HE Jia-heng;MENG Rui-bo;WU Chuan;WU Bang-hua(Guangdong Provincial Institute for Prevention and Control of Occupational Disease,Provincial Key Laboratory of Occupational Disease Prevention and Treatment,Guangzhou,Guangdong 510300,China)
出处
《中国职业医学》
CAS
北大核心
2022年第4期425-428,共4页
China Occupational Medicine
基金
广东省自然科学基金(2020A1515010893)
广东省职业病防治重点实验室(2017B030314152)
关键词
工作场所
空气
硫酸二甲酯
硅胶管
柱前衍生
高效液相色谱
测定
Workplace
Air
Dimethyl sulfate
Silicone tube
Pre-column derivatization
High performance liquid chromatography
Determination
