自动顶空进样—气相色谱法测定柠檬酸中溶剂残留

Determination of Residual Solvents in Citric Acid by Gas Chromatography with Automatic Headspace Sampling

[目的]建立自动顶空进样—气相色谱法测定柠檬酸中5种溶剂残留的分析方法。[方法]样品用水溶解,自动顶空进样,氢火焰检测器（FID）检测,外标法定量。[结果]平均回收率为85%~101%,相对标准偏差（RSD）为1.7%~4.2%,二氯甲烷、氯仿、苯、三氯乙烯、二氧六环检出限（LOD）分别为2、1、0.05、1、8mg/kg。[结论]该方法简便、快速、灵敏、准确,适合柠檬酸中5种溶剂残留定性和定量测定。

A method for determination of five residual solvents in citric acid by gas chromatography with automatic headspace sampling has been developed.Sample was extracted with water.Automatic headspace sampler and flame ionization detector（FID） were employed.External standards were used for quantitative determination.The average recoveries were 85%-101% and relative standard deviations were 1.7%-4.2%.The limit of detection were 2,1,0.05,1 and 8mg/kg for methylene chloride,chloroform,benzene,trichloroethylene and 1,4-dioxane respectively.The method was simple,rapid,sensitive and accurate,it was suitable for the quantitative determination and confirmation of five residual solvents in citric acid.