固相萃取-高效液相色谱法测定纺织品中的有害抗菌剂  

Determination of four antibacterial agents from textiles by solid phase extraction with high performance liquid chromatography

作　　者：徐韵扬 秦鑫[1] 顾虎[1] 胡喆[1] 王敏超 吴怡 XU Yunyang;QIN Xin;GU Hu;HU Zhe;WANG Minchao;WU Yi(Hangzhou Institute of Test and Calibration for Quality and Technology Supervision,Hangzhou,Zhejiang 310019,China)

机构地区：[1]杭州市质量技术监督检测院,浙江杭州310019

出　　处：《毛纺科技》2020年第9期50-54,共5页Wool Textile Journal

基　　金：国家重点研发项目(2017YFF0209600);中国标准化研究院国家标准馆项目(JXJY-2017-266);浙江省质量技术监督系统科研项目(20190119)。

摘　　要：为了评估纺织品中有毒有害抗菌剂的风险等级,建立了固相萃取-高效液相色谱法(SPE-HPLC)测定纺织品中三氯卡班、α—溴肉桂醛、2—(4—噻唑)—苯并咪唑、4—氯—3—甲基苯酚4种有毒有害抗菌剂的分析方法。纺织品经甲醇-四氢呋喃提取后,经强阳离子固相萃取小柱净化,采用安捷伦Eclipse XDB-C 18色谱柱(长度150 mm,孔径4.6 mm,填充物粒径5μm),以体积比乙腈/水40/60为流动相,对目标物进行有效分离,采用DAD检测器检测,结合色谱保留时间和光谱图进行定性,以标准曲线定量。4种有毒有害抗菌剂在质量浓度为1.0~100.0 mg/L范围内线性良好,相关系数均大于0.999。以信噪比S/N为10计算,该方法的定量限为2.2~3.6 mg/kg。在添加水平为5~100 mg/kg时,回收率为86.5%~100.3%,相对标准偏差为1.9%~4.3%。A novel method was established to determine trichlorocaban,α—bromocinnamaldehyde,2—(4—thiazole)—1H—benzimidazole and 4—chloro—3—methylphenol in textiles by solid phase extraction(SPE)with high performance liquid chromatography(HPLC)for evaluating the risk level of toxic and harmful antibacterial agents in textiles.The antibacterial agents were extracted from textiles with methanol-tetrahydrofuran,purified by strong cation exchange(SCX)SPE colume,and analyzed by HPLC-DAD on a Agilent Eclipse XDB-C 18 column(150 mm×4.6 mm,5μm),employing acetonitrile-water with a volume ratio of 40/60 as the mobile phase in a gradient elution mode.The antibacterial agents were qualitatively determined by retention time,and confirmed by ultraviolet spectrum.Under the optimal conditions,the target analytes were in range of 1.0-100.0 mg/L with the correlation coefficients higher than 0.999,and the method limits of quantification of target analytes were from 2.2 mg/kg to 3.6 mg/kg when the signal to noise ratio is 10.The spiked recoveries were in the range between 86.5%and 100.3%,and relative standard deviation ranged from 1.9%to 4.3%.The method is simple,precise and has high recoveries for the determination of antibacterial agents in textiles.

关 键 词：抗菌剂 固相萃取 高效液相色谱法 纺织品检测 

分 类 号：TS195.583[轻工技术与工程—纺织化学与染整工程]