超声萃取–气相色谱–质谱法同时测定皮革制品中11种氯甲苯类化合物

建立了皮革制品中2-一氯甲苯、3-一氯甲苯、4-一氯甲苯、2,4-二氯甲苯、2,5-二氯甲苯、2,6-二氯甲苯、2,3-二氯甲苯、3,4-二氯甲苯、2,3,6-三氯甲苯、2,4,5-三氯甲苯、五氯甲苯等11种氯甲苯类化合物的超声萃取–气相色谱–质谱分析方法。样品用二氯甲烷溶液超声提取,提取溶液直接进气相色谱–质谱联用仪进行分析,以2,4,5,6-四氯间二甲基苯酚为内标物,内标法定量。11种氯甲苯类化合物的线性范围为0.1~2.0μg/m L,相关系数(r~2)不小于0.999 1,方法的定量限为0.1 mg/kg,加标回收率在79.7%~104.1%之间,测定结果的相对标准偏差小于8.0%(n=6)。该方法快速、简便,定性定量准确,灵敏度高,适用于皮革制品中11种氯甲苯类化合物含量的日常检测。

Simultaneous Determination of 11 Kinds of Chlorotoluene in Leather Products by Ultrasonic Extraction-Gas Chromatography-Mass Spectrometry

A method for determination of 11 kinds of chlorotoluene (2-chlorotoluene, 3-chlorotoluene, 4-chlorotoluene, 2,4-dichlorotoluene, 2,5-dichlorotoluene, 2,6-dichlorotoluene, 2,3-dichlorotoluene, 3,4-dichlorotoluene, 2,3,6-trichlorotoluene, 2,4,5-trichlorotoluene, pentachlorotoluene) in leather products was developed by ultrasonic extraction-gas chromatography-mass spectrometry (GC-MS). The sample was extracted with dichloromethane by ultrasonic, and the extract was determined by GC-MS with 2,4,5,6-tetrachloro-m-xylene as internal standard, and quantified by internal standard method. The linear calibration curve was obtained in the range of 0.1-2.0 μg/mL with the correlation coefficient (r2) not less than 0.9991. The limits of quantification (LOQs) were 0.1 mg/kg, the average recoveries were in the range of 79.7%-104.1% with the relative standard deviations below 8.0%(n=6). The method is rapid, simple, accurate qualitative and quantitative, high sensitivity, and it can be used in the daily determination of 11 chlorotoluene in leather products with satisfactory results.