中国皮革

2019, v.48;No.755(11) 21-25

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皮革中4种防霉剂含量的HPLC测定
Determination of four preservatives in leather by HPLC

章爱琴;马贺伟;郑漫辉;
ZHANG Aiqin;MA Hewei;ZHENG Manhui;College of Material and Textile Engineering, Jiaxing College;

摘要(Abstract):

参照ISO 13365-2011中的内容,建立了皮革中4-氯-3-甲氧基苯酚(CMK)、邻苯基苯酚(OPP)、N-辛基异噻唑啉酮(OIT)以及苯噻氰(TCMTB)4种防霉剂成分含量的固相萃取净化、液相色谱(HPLC)测定方法。样品采用超声波辅助乙腈萃取1次、时间60 min,2 mL萃取液经过Florisil固相萃取柱净化后进行HPLC测试;HPLC检测时,4种成分的检测波长均为280 nm,采用乙腈/水=70/30(v/v)等梯度洗脱。方法定量检出限10~35 mg/kg,回收率84.8%~98.7%。实际检测结果表明,所测的皮革中通常含有该4种防霉剂中的一种,其中以TCMTB最普遍。
Based on the standard ISO 13365-2011, the determination method of solid phase extraction purification and high performance liquid chromatography of four preservatives including 4-chloro-3-methylphenol(CMK), o-phenyl-phenol(OPP), octhilinone(OIT) and thiocyanic-acid(TCMTB) used in leather was investigated. The targets were extracted using ultrasound enhanced acetonitrile extraction in one step within 60 min. 2 mL aliquot of the extracts was purified by solid phase extraction cartridge with Florisil frits.Quantitative tests were performed by HPLC with UV detection at 280 nm for CMK,OPP,OIT and TCMTB.The mobile phase was acetonitrile/water 70/30(v/v).Limits of quantification(LOQ) was at the range of 10~35 mg/kg,and recoveries ranged from 84.8% to 98.7%. Real sample tests present that more than one of the four preservatives were contained in leather, and TCMTB dominates.

关键词(KeyWords): 皮革;防霉剂;液相色谱;检测;超声波萃取;固相萃取净化
leather;preservative;HPLC;test;ultrasonic extraction;solid phase extraction purification

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基金项目(Foundation): 嘉兴市皮革和纺织品染整清洁生产创新团队研究项目

作者(Author): 章爱琴;马贺伟;郑漫辉;
ZHANG Aiqin;MA Hewei;ZHENG Manhui;College of Material and Textile Engineering, Jiaxing College;

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