检测工作场所空气中异佛尔酮的溶剂解吸气相色谱法的改进  

Improvement of Solvent Desorption Method Applied for Isophorone in Workplace Air by Gas Chromatography

作　　者：沈朝烨[1] 温忆敏[1] 

机构地区：[1]上海市疾病预防控制中心卫生检测室,上海200336

出　　处：《环境与职业医学》2015年第2期164-167,共4页Journal of Environmental and Occupational Medicine

摘　　要：[目的]使用混合溶剂提高空气中异佛尔酮的溶剂解吸气相色谱测定法中的解吸效率。[方法]活性炭管采样后，10％（体积分数）异丙醇一二硫化碳混合溶剂解吸，聚乙二醇石英弹性毛细管柱INNOWAX（30．0m×0．53mm×1．0μm）分离，火焰离子化检测器检测，保留时间定性、标准曲线外标法定量。[结果]10％异丙醇一二硫化碳混合溶剂解吸活性炭中异佛尔酮，平均解吸效率为92．6％。浓度分别为10、60、150mg／L的异佛尔酮加标样品测定结果显示批内、批间相对标准偏差分别〈5％、10％。异佛尔酮在0．28～400mg／L呈线性关系，回归方程y=1．947x-0．904，相关系数r=1．0000；方法检出限为0．084mg／L。以2．5L采样量计算，异佛尔酮的最低检出浓度为0．034mg／m3，最低定量浓度为0．11mg／m3。[结论]采用10％异丙醇一二硫化碳混合溶剂为解吸剂，其解吸效率高于仅使用二硫化碳（〈70％）。该方法应用于工作场所空气中异佛尔酮的测定，方法精密度、准确度良好，解吸效率满足相关国家标准要求。[ Objective ] To improve the desorption efficiency in the determination of isophorone in workplace air by gas chromatography using mixed solvent. [ Methods ] Air samples collected with charcoal tubes were desorbed with 10% isopropanol and carbon disulfide mixture, separated with capillary column INNOWAX （30.0 m× 0.53 mm ×1.0 μm）, and detected with flame ion detector using retention time for qualification and external standard curve for quantitation of isopropanol. [ Results ] The 10% isopropanol and carbon disulfide mixture was applied for isophorone desorption, and the average desorption efficiency was 92.6%. The relative standard deviation of three isophorone spiked levels （10, 60, and 150 mg/L） was below 5% for intra assay or below 10% for inter assay. A good linearity was observed in the range of 0.28-400mg/L with the regression equation y=1.947x-0.904 and correlation coefficient r=-1.0000. The limit of detection of the method was 0.084 mg/L. The minimum detectable concentration and the limit of quantitation of isophorone in solvent and air were 0.034 mg/m3 and 0.11 mg/m3 respectively based on sampling volume （2.5 L）. [ Conclusion ] The method using 10% isopropanol and carbon disulfide mixture as desorption solvent for determination of isophorone in workplace air is of great precision and accuracy. Its desorption efficiency is higher than the method using carbon disulfide only （〈70%） and meets the requirements of relative standards.

关 键 词：异佛尔酮 工作场所空气 气相色谱法 溶剂解吸 

分 类 号：R115[医药卫生—公共卫生与预防医学]