摘要
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.
作者
冯徐根
白子竹
蔚彪
韩军
杨萌
FENG Xugen;BAI Zizhu;YU Biao;HAN Jun;YANG Meng(Beijing Product Quality Supervision and Inspection Institute,National Textile and Leather Products Quality Supervision Texting Center,Beijing 100025,China)
出处
《中国皮革》
CAS
2021年第10期137-143,共7页
China Leather
关键词
防霉剂
气质联用仪
液相色谱仪
preservatives
gas chromatography-mass spectrometry(GC—MS)
liquid chromatography