摘要
文章建立了高效液相色谱–串联质谱法测定家具用皮革中2,4–二氨基甲苯和4,4′–二氨基二苯甲烷含量的分析方法。试验选用Shim–pack GIST–HP C_(18)色谱柱进行分离,以0.005 mol/L乙酸铵水溶液–甲醇为流动相进行洗脱,流速为0.3 mL·min^(−1)。质谱分析中采用电喷雾离子源及多反应监测模式,外标曲线法定量。结果表明,2,4–二氨基甲苯和4,4′–二氨基二苯甲烷在50~500μg/L质量浓度范围内具有良好的线性关系,相关系数R^(2)均>0.999。2,4–二氨基甲苯和4,4′–二氨基二苯甲烷检出限分别为2.13μg/kg和0.18μg/kg,定量限分别7.03μg/kg和0.53μg/kg,相对标准偏差(n=6)分别为4.75%~7.14%和2.93%~6.84%,在3个加标水平下的平均回收率分别为88.69%~93.74%和91.47%~96.84%,该方法简单快速、灵敏度高、准确可靠,适用于家具用皮革中2,4–二氨基甲苯和4,4′–二氨基二苯甲烷的检验检测。
This article established an analytical method for determining the contents of 2,4-diaminotoluene(TDA)and 4,4'-diaminodiphenylmethane(MDA)in furniture leather using high performance liquid chromatography-tandem mass spectrometry.The experiments used a Shim-pack GIST-HP C_(18)chromatographic column for separation,and 0.005 mol/L ammonium acetate aqueous solution-methanol was adopted as the mobile phase for elution at a flow rate of 0.3 mL min^(−1).The electrospray ion source and multi-reaction monitoring mode were used in the mass spectrometry analysis,and the external standard curve method was used for quantification.The results showed that there was a good linear relationship for TDA and MDA in the mass concentration range of 50–500μg/L with the correlation coefficients R^(2)>0.999.The detection limits of TDA and MDA were 2.13μg/kg and 0.18μg/kg,respectively,and their quantification limits were 7.03μg/kg and 0.53μg/kg,respectively,while the relative standard deviations(RSD,n=6)were 4.75%–7.14%and 2.93%-6.84%,respectively,and the average recovery rates at three spiked levels were 88.69%-93.74%and 91.47%-96.84%,respectively.This method is simple,fast,sensitive,accurate and reliable,and is suitable for the detection of TDA and MDA in furniture leather.
作者
张琴
杨星华
王淳璐
许倩
李加涛
余宏
ZHANG Qin;YANG Xinghua;WANG Chunlu;XU Qian;LI Jiatao;YU Hong(Chengdu Product Quality Inspection and Research Institute Co.,Ltd,Chengdu 610100,China;Chengdu Research Institute of Product Quality Supervision and Inspection,Chengdu 610100,China)
出处
《皮革科学与工程》
北大核心
2025年第6期64-68,共5页
Leather Science and Engineering
