摘要
采用加速溶剂萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS),建立了一种快速提取和测定纺织品中8种二苯甲酮类防紫外线整理剂的分析方法。样品经提取、浓缩,甲醇定容,采用Acquity UPLC?BEH C18柱分离,以乙腈-0.05%甲酸水溶液为流动相,梯度洗脱,电喷雾正负离子模式多反应监测,外标法定量。该方法在0.05~0.70μg/m L范围内线性关系良好(R>0.99),在添加质量浓度分别为0.5、1.0和2.0 mg/kg时,棉布样品平均回收率范围为(89.53±2.20)%^(99.52±4.06)%,相对标准偏差(RSD)为2.03%~5.46%;涤纶样品平均回收率范围为(96.74±6.33)%^(107.23±7.64)%,相对标准偏差(RSD)为3.01%~7.69%;尼龙样品平均回收率范围为(93.99±5.45)%^(111.33±3.45)%,相对标准偏差(RSD)为1.17%~7.11%,方法检出限(LOD)为0.24~3.43μg/kg,方法定量限(LOQ)为0.80~11.44μg/kg。
A novel method has developed for the rapid extraction and determination of 8 diphenyl ketone anti-ultraviolet finishing agents in textiles by accelerated solvent extraction （ASE） coupled with ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. The analytics in the textiles are extracted by ASE and dried by rotavapor, then redissolved in methanol. The chromatographic analysis is performed on an Acquity UPLC BEH C18 column by a gradient elution employing of acetonitrile and 0.05% formic acid as a mobile phase. The analytics are detected by electrospray ionization （ESI） tandem mass spectrometry with multiple reaction monitoring （MRM） in positive and negative ion mode simultaneously. Good linearity （R〉 0.99） is observed between 0.05N0.70 μg/mL for all compounds. The recoveries and relative standard deviations （RSDs） are checked by spiking untreated samples with the 8 analysts at 0.5, 1.0 and 2.0 mg/kg. The average recoveries of the 8 compounds in the cotton, terylene and nylon samples are （89.53±2.20）%～（99.52±4.06）%, （96.74±6.33）%～（107.23±7.64）% and （93.99±5.45）%～ （111.33±3.45）%, respectively. The RSDs are 2.03%-5.46%, 3.01%-7.69% and 1.17%～7.11% （n =6）, respectively. The limits of detection are 0.24N3.43μg/kg, and the limits of quantification are 0.80～11.44 μg/kg for the 8 analytics.
出处
《印染》
北大核心
2016年第22期37-41,共5页
China Dyeing and Finishing
基金
国家质检总局科研项目(2015IK305)
关键词
测试
加速溶剂萃取
超高效液相色谱
串联质谱
二苯甲酮类防紫外线整理剂
纺织品
testing
accelerated solvent extraction
ultra performance liquid chromatography
tandem mass spectrometry
diphenyl ketone anti-ultraviolet finishing agents
textiles
