皮革中异噻唑啉酮防霉剂的检测方法  

Detection Methods of Isothiazolinone Fungicides in Leather

作　　者：林芳 毛树禄 陈斌 余鹏飞[2] 李正军[2] 

机构地区：[1]晋江出入境检验检疫局国家鞋类检测中心,福建晋江362200 [2]四川大学制革清洁技术国家工程实验室,四川成都610065

出　　处：《中国皮革》2011年第7期5-10,共6页China Leather

基　　金：国家质检总局科研项目(2010IK100)资助

摘　　要：采用HPLC-DAD和GC-MS研究并优化皮革中主要异噻唑啉酮类防霉剂的检测方法。结果表明:以甲醇为溶剂,采用HPLC-DAD法检测异噻唑啉酮含量在检出限及响应值方面优于GC-MS法,HPLC-DAD检测优化条件:流动相V(甲醇)∶V(水)为35∶65,柱温30℃,流速0.6mL/min,进样体积15μL。当标样的浓度为0.625～10mg/L时,线性相关系数≥0.9998,MI、CMI和BI的检出限分别为0.026、0.054和0.122mg/L。当取样量为0.5g时,超声波萃取法对皮革阳性样品的优化萃取条件为溶剂甲醇30mL,萃取时间10min,萃取温度30℃,超声频率40kHz。空白样品的加标回收率为91.7%～98.7%,标准储备液(-18℃)和标准工作液(-4℃)在避光条件下可稳定存放60d。In order to tackle the update international regulation,the analysis methods of major isothiazolinone fungicides widely used in leather making process,namely,2-methyl -3-isothiazolinone（ MI） ,5-chloro-2-methyl-3-isothiazolinone （ CMI） and 1, 2-benzisothiazolinone （ BI） ,were studied. The analyzing methods of MI,CMI and BI were investigated with methanol as selected solvent. The results indicate that the detection of isothiazolinone fungicides by HPLC-DAD could gain better results comparing that by GC-MS,with lower detection limit and high responsively. The optimized HPLC-DAD analyzing procedure to aim isothiazolinone is as follow： fluent phase V（ water）∶V（ methanol） 65∶35,column temperature 30℃ , flow velocity 0. 6mL/min,and sample volume 15μL. The peak area and the concentration of MI,CMI and BI shows excellent linearity when the concentration of them is about 0. 625～10mg/L,with the related coefficient is above 0. 999 8. The detection limits of MI,CMI and BI are 0. 026mg/L、 0. 054mg/L and 0. 122mg/L respectively. Leather samples could be extracted by ultrasonic machines,with 30mL methanol as solvent,extracting for 10min,and supersonic frequency of 40kHz at 30℃ . In order to ensure the precision and accuracy of the detection experiment,recoveries of the standard working solution with various concentrations in blank samples were researched and the results are 91. 7%～98. 7% . The stabilities of the standard stock solution at-18℃ and standard working solution at-4℃ under the dark conditions were determined and both of them would be preserved for at least 60 days.

关 键 词：皮革 异噻唑啉酮 检测方法 HPLC-DAD 超声萃取 

分 类 号：TS57[轻工技术与工程—皮革化学与工程]