超声萃取-气相色谱法同时测定皮革及其制品中21种有害有机溶剂的残留量

Simultaneous Determination of the Residual Contents of 21 Harmful Organic Solvents in Leather and Leather Products by Gas Chromatography Combined with Ultrasonic Extraction

建立了一个能同时测定皮革及其制品中21种有害有机溶剂残留量的气相色谱方法,该方法以乙酸乙酯为提取溶剂,45℃下超声提取皮革及其制品中残留的有害有机溶剂,提取液经固相萃取柱净化后进行气相色谱-火焰离子检测器（GC-FID）分析,外标法定量。该方法操作简单,定量准确,检出限低,各组分的检出限为0.05-0.50 mg/kg,在3个不同加标水平下,加标平均回收率为81.13%-96.47%,精密度实验RSD为3.11%-4.71%（n=9）。采用该方法对512个市售皮革样品进行测定,在39个样品中检出不同含量水平的多种目标分析物。

An effective gas chromatographic method was established for the simultaneous determination of the residual contents of 21 harmful organic solvents in leather and leather products.Harmful organic solvents in leather and leather products were ultrasonically extracted at 45℃, using ethyl acetate as the extraction solvent. The extract was then purified by solid-phase extraction column,followed by the analysis of gas chromatography-flame ionization detector（GC-FID） technique. The concentration of each analyte were calibrated by external standard method. The proposed method was simple, accurate and sensitive. The limits of detection（LODs） varied from 0.05mg/kg to 0.50mg/kg.The spiked average recoveries varied from 81.13% to 96.47% under three different spiked levels while the relative standard deviation（RSD） changed from 3.11% to 4.71%. The proposed method was applied to the analysis of 512 commercially available leather and leather product samples and some target compounds at different content levels were detected in 39 samples.