论文部分内容阅读
建立了高效液相色谱-串联质谱(HPLC-MS/MS)联用技术同时测定纺织品和皮革中10种酚类化合物的方法。样品经甲醇超声提取、浓缩后,经Oasis HLB固相萃取柱净化,采用Eclipse Extend-C18色谱柱(2.1 mm×100mm,3.5μm),乙腈和0.01 mol/L甲酸铵水溶液(pH=6.3)为流动相梯度洗脱,电喷雾离子源电离,负离子多反应监测模式进行定性和定量分析。10种酚类化合物在0.08~5 mg/L浓度范围内与峰面积呈良好的线性关系,相关系数为0.9931~0.9993;以不低于3倍的信噪比计算10种酚类化合物的检出限(LOD)为0.0001~0.0034 mg/kg;定量限(LOQ,S/N≥10)为0.0005~0.0113 mg/kg。棉、麻、毛、皮革4种基质在3个不同加标水平的回收率为77%~108%,相对标准偏差(RSDs)为1.7%~10.8%。该方法能同时完成10种酚类化合物的确证和分析,适用于纺织品和皮革中酚类化合物残留的检测分析。
A method for simultaneous determination of ten phenolic compounds in textiles and leather by HPLC-MS / MS was established. The sample was extracted by methanol and concentrated. The sample was purified by Oasis HLB solid phase extraction. The column was eluted with Eclipse Extend-C18 column (2.1 mm × 100 mm, 3.5 μm), acetonitrile and 0.01 mol / L ammonium formate Mobile phase gradient elution, electrospray ionization ionization, anion multi-reaction monitoring mode for qualitative and quantitative analysis. The 10 phenolic compounds showed a good linear relationship with the peak area in the concentration range of 0.08-5 mg / L with the correlation coefficient of 0.9931-0.9993. The detection of 10 phenolic compounds was carried out with no less than 3 times the signal to noise ratio The limits of quantification (LOD) ranged from 0.0001 to 0.0034 mg / kg. The limits of quantification (LOQ, S / N≥10) ranged from 0.0005 to 0.0113 mg / kg. The recoveries of cotton, hemp, wool and leather at three different spiked levels ranged from 77% to 108% and the relative standard deviations (RSDs) ranged from 1.7% to 10.8%. The method can simultaneously confirm and analyze 10 kinds of phenolic compounds and is suitable for the detection and analysis of phenolic compounds residues in textiles and leather.