鞋类皮革部件中苯二胺类物质的HPLC-MS/MS测定方法
Determination of Phenylenediamines in Footwear Leather Components by HPLC-MS/MS
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摘要: 建立了鞋类皮革部件中对苯二胺、邻苯二胺和间苯二胺含量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。该法以甲醇为溶剂进行二次超声提取,净化后的提取液进行HPLC-MS/MS测定,外标法定量。试验结果表明:在5~500 μg/L质量浓度范围内,三种苯二胺的线性相关系数均大于0.997,线性关系良好;在该方法的试验条件下,三种苯二胺的检出限为0.02~0.03 mg/kg,平均加标回收率在89%~106%范围内,相对标准偏差在3%~9%之间。该方法可用于鞋类皮革部件中对苯二胺、邻苯二胺和间苯二胺残留量的检测分析。Abstract: A method for determining the content of p-phenylenediamine, o-phenylenediamine and m-phenylenediamine in footwear leather components was established by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method. Ultrasonic treatment was carried out for two times using methanol as solvent. Then the purified extracting solution was analyzed by HPLC-MS/MS and quantified by external standard method. The results showed that the linearly dependent coefficients of 3 kinds of phenylenediamines are all above 0.9997 in the concentration range of 5-500 μg/L, demonstrating good linear relationships. According to the condition of this study, the detection limits of 3 kinds of phenylenediamines are 0.02-0.03 mg/kg, and the average recovery ratios ranged from 89% to 106%, while the relative standard deviations of 3%-9% were obtained. The developed method was applicable for the determination of p-phenylenediamine, o-phenylenediamine and m-phenylenediamine residues in footwear leather components.