| 超声萃取结合超高效液相色谱法测定皮革中10种防霉剂 |
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| 基金项目: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） |
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| 中文摘要: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（r2）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。 |
| 中文关键词:皮革 防霉剂 超声萃取 超高效液相色谱（UPLC） |
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| Determination of 10 Kinds of Fungicides in Leather by Ultrasonic Extraction Combined with Ultrahigh Performance Liquid Chromatography |
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| Abstract: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. |
| Key Words:leather fungicide ultrasonic extraction ultrahigh performance liquid chromatography（UPLC） |
| 引用本文：吴玉銮*，王莉，罗海英，冼燕萍，董浩，王斌，韩婉清.超声萃取结合超高效液相色谱法测定皮革中10种防霉剂[J].分析测试学报,2016,35(9):1116-1120. |
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