气相色谱质谱联用法测定皮革及毛皮中4种防霉剂

Determination of 4 preservatives in leather and fur by gas chromatography-mass spectrometry(GC-MS)

建立了气相色谱质谱联用法测定皮革和毛皮中防霉剂的分析方法,以乙腈为萃取溶剂,采用超声萃取法提取皮革和毛皮中的对氯间甲酚(PCMC)、邻苯基苯酚(0PP)、辛噻酮(0IT)、苯噻氰(TCMTB)4种防霉剂,优化了样品前处理条件和仪器分析条件。方法线性范围0.5~20μg/mL,方法检出限5.0~8.0 mg/kg,加标回收率88.4%~95.7%,相对标准偏差3.2%~6.1%。本方法与液相色谱法同时测定实际样品中的防霉剂结果偏差矣15%,结果一致性较好。市售的皮革和毛皮测定结果显示,检出率为45.7%,检出样品中普遍含有1~3种防霉剂,PCMC检出率最高,TCMTB检出结果最大。

The measuring method for the determination of preservatives in leather and fur by GC-MS was established.Acetonitrile was used as the extraction solvent and ultrasonic extraction was used to extract four preservatives including 4-chloro-3-methylphenol(PCMC),o-phenylphenol(OPP),octhilinone(OIT)and benthienyl(TCMTB)in leather and fur,the sample pretreatment conditions and instrument analysis conditions were optimized.The linear range of the method is 0.5〜20μg/mL,method detection limit is at the range of 5.0〜8.0 mg/kg,the recover-ies range from 88.4%to 95.7%,and the relative standard deviation is at the range of 3.2%〜6.1%.The detection results deviation of the 4 preservatives in the real samples by less than 15%between this method and liquid chromatography method,and the results are consistent.The testing results of commercial samples show the detection rate is 45.7%,and generally 1〜3 kinds of preservatives are contained in detected samples.PCMC has the highest detection rate and TCMTB has the largest detection result.