超声萃取结合超高效液相色谱法测定皮革中10种防霉剂  

Determination of 10 Kinds of Fungicides in Leather by Ultrasonic Extraction Combined with Ultrahigh Performance Liquid Chromatography

作　　者：吴玉銮[1,2] 王莉[1,2] 罗海英[1,2] 冼燕萍[1,2] 董浩[1,2] 王斌[1,2] 韩婉清[1,2] 

机构地区：[1]广州质量监督检测研究院,广东广州511447 [2]国家皮革制品质量监督检验中心(广州),广东广州511447

出　　处：《分析测试学报》2016年第9期1116-1120,共5页Journal of Instrumental Analysis

基　　金：广东省质量技术监督局科技项目(2015PZ06);广州市质量技术监督局科技项目(2015kj10)

摘　　要：建立了皮革样品中10种防霉剂(氨基苯磺酰胺、苯并咪唑、BIT、MBT、IPBC、PCMC、水杨酰苯胺、OPP、TCMTB和OIT)的超高效液相色谱(UPLC)检测方法。样品经甲醇超声萃取,T3色谱柱分离后,甲醇和0.1%甲酸水为流动相梯度洗脱,二极管阵列检测器测定。在优化条件下,10种防霉剂在一定的浓度范围内线性关系良好,相关系数(r^2)均不小于0.999 3,除IPBC的方法定量下限(S/N=10)为190.0 mg/kg外,其余9种防霉剂的方法定量下限为4.0~8.0 mg/kg,平均回收率为81.3%~104.9%,相对标准偏差(RSD,n=6)为4.7%~11.2%。该方法前处理简单、分离效果好,适用于皮革样品中10种防霉剂的同时测定。A new method was established to determine 10 kinds of fungicides（including sulfanilamide，benzimidazole，BIT，MBT，IPBC，PCMC，salicylanilide，OPP，TCMTB，OIT） in leather samples by ultrasonic extraction combined with ultrahigh performance liquid chromatography（UPLC）.The leather samples were ultrasonically extracted with methanol，and separated with T3 column，employing methanol and 0.1%（by volume） formic water as mobile phase by gradient elution．All of the samples were detected with diode-array detector.The 10 kinds of analytes presented favorable linearity in a certaim concentration range，with correlation coefficients（r2） not less than 0.999 3.The method quantitation limit（LOQ，S/N=10） of IPBC was 190.0 mg/kg，and the LOQs of other compounds were in the range of 4.0-8.0 mg/kg.The average recoveries（n=6） ranged from 81.3% to 104.9%，and the relative standard deviations （RSD，n=6） were in the range of 4.7%-11.2%.With the advantages of simple pre-treatment procedure and satisfactory separate effect，the developed method was suitable for the simultaneous determination of 10 kinds of fungicides in leather samples.

关 键 词：皮革 防霉剂 超声萃取 超高效液相色谱(UPLC) 

分 类 号：O657.72[理学—分析化学] TQ572.41[理学—化学]