工作场所空气中草酸二甲酯和草酸二乙酯同时测定的高效液相色谱法  

Determination of dimethyl oxalate and diethyl oxalate in workplace air by high performance liquid chromatography

作　　者：陈志亮 王敏 江金凤 宋为丽 Chen Zhiliang;Wang Min;Jiang Jinfeng;Song Weili(Health Laboratory,Wuhan Prevention and Treatment Center for Occupational Diseases,Wuhan 430015,China)

机构地区：[1]武汉市职业病防治院卫生检验科,武汉430015

出　　处：《中华劳动卫生职业病杂志》2024年第3期199-202,共4页Chinese Journal of Industrial Hygiene and Occupational Diseases

基　　金：中国疾病预防控制中心公共卫生领域卫生健康标准化前期研究项目(BZ2022-Q017)。

摘　　要：目的建立工作场所空气中草酸二甲酯(DMO)和草酸二乙酯(DEO)同时测定的高效液相色谱检测方法。方法于2022年1月至2023年1月, 空气样品采用硅胶管采集, 乙腈洗脱解吸, 经C18色谱柱分离, 二极管阵列检测器检测, 在210 nm波长下, 以保留时间定性, 峰面积定量。结果 DMO和DEO测定方法的线性关系良好, r>0.999。DMO和DEO的方法检出限分别为0.39 μg/ml、0.52 μg/ml, 方法定量下限分别为1.28 μg/ml、1.72 μg/ml。DMO和DEO的平均解吸效率分别为82.40%~92.72%、94.13%~97.69%, 批内精密度分别为1.87%~6.18%、2.25%~3.31%, 批间精密度分别为3.29%~5.73%、1.38%~2.94%。平均采样效率均为100%。DMO穿透容量为37.61 mg(200 mg固体吸附剂), DEO穿透容量为>28.11 mg(200 mg固体吸附剂)。在4 ℃条件下样品至少可以保存7 d。结论该方法操作简便、实用性强, 各项指标均满足规范要求, 适用于工作场所空气中DMO和DEO的同时测定。Objective To establish a high performance liquid chromatography method for the simultaneous determination of dimethyl oxalate(DMO)and diethyl oxalate(DEO)in workplace air.Methods From January 2022 to January 2023,air samples were collected by silica gel tubes,desorbed by acetonitrile,separated by C18 chromatographic column,detected by photo-array detector,and retention time was used to characterize and peak area was used to quantify at 210 nm wavelength.Results The linear relationships of DMO and DEO were good,r>0.999.The detection limits of DMO and DEO were 0.39 and 0.52μg/ml,respectively.The quantitative limit was 1.28μg/ml for DMO and 1.72μg/ml for DEO.Average desorption efficiency for DMO was 82.40%-92.72%,and DEO was 94.13%-97.69%.The intra-assay precision of DMO was 1.87%-6.18%,and DEO was 2.25%-3.31%.Inter-assay precision of DMO was 3.29%-5.73%,and DEO was 1.38%-2.94%.Average sampling efficiencies were 100%for both DMO and DEO.Breakthrough capacity of DMO was 37.61 mg(200 mg solid adsorbent),DEO was>28.11 mg(200 mg solid adsorbent).Samples should be stored at 4℃for at least 7 days.Conclusion This method is easy to operate and has strong practicability.All indicators meet the requirements of the specification,and it is suitable for the simultaneous determination of DMO and DEO in the workplace air.

关 键 词：工作场所 草酸二甲酯 草酸二乙酯 高效液相 色谱法 空气 

分 类 号：R134.4[医药卫生—劳动卫生] O657.72[医药卫生—公共卫生与预防医学]