超声萃取UPLC-MS/MS测定纺织品中水杨酸酯类防紫外线整理剂  

Determination of Salicylate Anti-ultraviolet Finishing Agents in Textiles by UPLC-MS/MS Coupled with Ultrasonic Extraction

作　　者：吴刚 虞慧芳[2] 何坚刚 席广成[3] 王力君 张明誉 应苏玲 WU Gang;YU Huifang;HE Jiangang;XI Guangcheng;WANG Lijun;ZHANG Mingyu;YING Suling(Zhejiang Academy of Inspection & Quarantine of Science & Technology, Hangzhou, Zhejiang, 311215, China;Zhejiang Academy of Agricultural Sciences;China Academy of Inspection and Quarantine;Zhejiang Lead Product Technology Co. Ltd.)

机构地区：[1]浙江省检验检疫科学技术研究院,浙江杭州311215 [2]浙江省农业科学院 [3]中国检验检疫科学研究院 [4]浙江立德产品技术有限公司

出　　处：《检验检疫学刊》2019年第4期6-11,共6页Journal of Inspection and Quarantine

基　　金：浙江省公益研究计划项目(LGG18B070001);国家重点研发计划(2017YFF0210003)

摘　　要：利用超声萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)检测技术,建立了一种快速提取和测定纺织制品中7种水杨酸酯类防紫外线整理剂(水杨酸苯酯、水杨酸-p-叔丁基苯酯、水杨酸-p-叔辛基苯酯、间苯二酚单苯甲酸酯、对-二甲基氨基苯甲酸-2-乙基己酯、水杨酸-2-乙基己酯、水杨酸三甲环己酯)的分析方法。样品经超声提取、净化,采用Acquity UPLCR ■HSS T3柱(2.1mm×100mm,1.8μm)分离,以乙腈-水溶液为流动相,梯度洗脱,电喷雾正、负离子模式电离,多反应监测模式检测,外标法定量。该方法在0.1~1.0μg/mL时线性关系良好(r>0.99)。在添加浓度为5.0~20.0mg/kg时,棉布样品的平均回收率为85.32%~105.45%,相对标准偏差(RSD)为2.57%~9.15%;涤纶样品的平均回收率范围为89.81%~104.36%,相对标准偏差(RSD)为3.26%~8.34%;尼龙样品的平均回收率范围为84.56%~105.86%,相对标准偏差(RSD)为1.46%~9.92%,方法检出限(LOD)为0.02~0.2mg/kg,方法定量限(LOQ)为0.06~0.6mg/kg。该方法简单、快速,方法的最低检测限和添加回收率均满足纺织品中7种水杨酸酯类防紫外线整理剂的测定。This paper has developed a novel method to extract and determine 7 salicylate anti-ultraviolet finishing agents in textiles by ultrasonic extraction with methanol coupled with high performance liquid chromatography. The chromatographic analysis is performed on an Acquity UPLCR ■ HSS T3(2.1 mm×100 mm,1.8 μm) column by a ramped mobile phase. The analytes are detected by HPLC with DAD by external standard quantitative method. The recovery test results of seven kinds of salicylate anti-UV finishing agents on blank cotton, terylene and nylon samples.The experimental result shows that good linearity(r>0.99)is observed between 1.0-10.0 μg/mL for all compounds. The recoveries and relative standard deviations(RSD)are checked by spiking untreated samples with the 7 salicylate anti-ultraviolet finishing agents at 5.0, 10.0 and 20.0 mg/kg. The average recoveries of the 7 compounds in the cotton, terylene and nylon samples are from 85.32% to 105.45%, from 89.81% to 104.36% and from 84.56% to 105.86%, respectively. The precision values expressed as RSD are from 2.57% to 9.15%, from 3.26% to 8.34% and from 1.46% to 9.92%(n=6), respectively. The limits of detection range from 0.02 mg/kg to 0.2 mg/kg and the limits of quantification are from 0.06 mg/kg to 0.6 mg/kg for the 7 analytes. The results shows that the methodis simple and rapid, and the minimum detection limit and recovery rate of the method meet the requirements of the determination of 7 salicylate anti-ultraviolet finishing agents in textiles.

关 键 词：超声萃取 超高效液相色谱-串联质谱 纺织品 水杨酸酯防紫外线整理剂 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程]