摘要:
为监控皮革及其制品中有害有机溶剂的残留量,建立了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-串联质谱(GC-MS/MS)法。以乙酸乙酯为萃取溶剂,超声萃取皮革及其制品中残留的有害有机溶剂,萃取液经固相萃取柱净化后进行 GC-MS/MS 分析,外标法定量。结果表明,各组分的检出限为15~100μg/kg,平均加标回收率为80.6%~95.8%,精密度(RSD)为2.3%~6.7%(n=9)。采用该方法测定512个市售皮革制品中21种有机溶剂的残留量,在其中的55个样品中检出 N ,N-二甲基甲酰胺(DMF)、N ,N-二甲基乙酰胺(DMA)、乙二醇单乙醚(EGEE)、乙二醇单丁醚(EGBE)、二乙二醇单乙醚(DEGEE)、二乙二醇单丁醚(DEGBE)、三乙二醇单甲醚(TEGME)、三乙二醇单丁醚(TEGBE)、N-甲基吡咯烷酮(NMP)等9种目标分析物,其中检出率最高的是 DEGBE 和 DMF,检出含量最高的是 DEGBE。该方法快速简便、灵敏度高,适用于皮革及其制品中有害有机溶剂残留量的检测。
Abstract:
In order to monitor the residual contents of harmful organic solvents in leath-er and leather products,a method of gas chromatography-tandem mass spectrometry (GC/MS-MS)was established for the simultaneous determination of 21 harmful organic solvents.Residual harmful organic solvents in leather and leather products were ultra-sonically extracted using ethyl acetate as the extraction solvent,then the extract was purified by solid-phase extraction (SPE)column and was analyzed by GC-MS/MS.All the analyte were calibrated by the external method.The results show that the limits of quantification (LOQ)are 15 μg/kg for ethylene glycol diethyl ether (EGEE),ethylene glycol dibutyl ether (EGDBE)and N-methylpyrrolidone (NMP);the limit of quantifica-tion is 20 μg/kg for ethylene glycol methyl ether (EGME);the limits of quantification are 25 μg/kg for diethylene glycol dimethyl ether (DEGDME ), N ,N-dimethyl-formamide (DMF ),ethylene glycol butyl ether (EGBE ),N ,N-dimethylacetamide (DMA),N-methylformamide (MF)and diethylene glycol butyl ether (DEGBE);the limits of quantification are 50 μg/kg for ethylene glycol dimethyl ether (EGDME), ethylene glycol ethyl ether (EGEE),diethylene glycol methyl ether (DEGME),dieth-ylene glycol ethyl ether (DEGEE),N-methylacetamide (MA),triethylene glycol dime-thyl ether (TEGDME),formamide,triethylene glycol methyl ether (TEGME),trieth-ylene glycol ethyl ether (TEGEE)and triethylene glycol butyl ether (TEGBE);the lim-it of quantification is 100 μg/kg for diethylene glycol diethyl ether (DEGDEE).The spiked average recoveries are 80.6%-95.8% under three different spiked levels.The relative standard deviation (RSD)of precision experiment changes from 2.3% to 6.7%. By using this method,5 12 commercially available leather and leather product samples were detected and 9 target compounds such as DMF,DMA,EGEE,EGBE,DEGEE, DEGBE,TEGME,TEGBE and NMP were found to exist in 55 samples.The ratios of detection of DEGBE and DMF are the highest among these 9 target compounds.DEGBE is found to exist in 39 samples and DMF is found to exist in 30 samples.And the residual content of DEGBE is the highest,which reaches to 447.4 mg/kg.The method is simple,rapid and sensitive,which suits for determination of 21 harmful organic solvents in leather and leather products.
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