纺织品中紫外线吸收剂的快速筛查和确证

1)深圳出入境检验检疫局工业品检测技术中心,广东深圳 518067; 2)深圳大学化学与环境工程学院,广东深圳 518060; 3)深圳职业技术学院应用化学与生物技术学院,广东深圳 518055

分析化学; 超声萃取; 纺织品; 紫外线吸收剂; 超高效液相色谱; 静电场轨道阱高分辨质谱; 正交实验

Rapid screening and confirmation of ultraviolet absorbers in textiles
Wang Chengyun1, Liu Caiming1, Lin Junfeng1, Xie Tangtang1, Shen Yawen2, and Cui Wei3

Wang Chengyun1, Liu Caiming1, Lin Junfeng1, Xie Tangtang1, Shen Yawen2, and Cui Wei31)The Testing and Technology Center for Industrial Products, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518067, Guangdong Province, P.R.China2)College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, Guangdong Province, P.R.China3)School of Applied Chemistry and Biological Technology, Shenzhen Polytechnic, Shenzhen 518055, Guangdong Province, P.R.China

analytical chemistry; ultrasonic extraction; textiles; ultraviolet absorbers; ultra-high performance liquid chromatography; orbitrap high resolution mass spectrometry; orthogonal experiment

DOI: 10.3724/SP.J.1249.2017.03322

备注

建立一种筛查和确证纺织品中紫外线吸收剂的超高效液相色谱/静电场轨道阱高分辨质谱(ultra-high performance liquid chromatography/orbitrap high resolution mass spectrometry, UPLC/Orbitrap HRMS)分析方法,以甲醇为萃取溶剂,超声萃取纺织品中的紫外线吸收剂,萃取液经浓缩定容后进行UPLC/Orbitrap HRMS分析,利用提取离子色谱峰面积进行外标法定量.在Hypersil Gold色谱柱(100 mm×2.1 mm, 1.9 μm)上完成19种紫外线吸收剂的色谱分离,流动相为甲醇和水,采取梯度洗脱方式.质谱分析分别采用电喷雾正负离子(ESI+和ESI-)电离模式,在质荷比m/z为100~700范围内进行1级质谱全扫描.利用保留时间和准分子离子的精确质量数进行定性,利用数据依赖扫描模式获得的离子质谱图进行定性确证,19种紫外线吸收剂的质量数准确度误差均小于2×10-6.19种紫外线吸收剂的定量限为0.01~0.50 μg/kg,在3个不同加标水平下,方法的平均加标回收率为82.35%~94.58%,相对标准偏差为3.37%~9.98%.应用该方法对市售纺织品中紫外线吸收剂进行筛查,在1个样品中检出UV-327.

An effective method was established for rapid screening and confirmation of ultraviolet absorbers in textiles by ultra-high performance liquid chromatography/orbitrap high resolution mass spectrometry(UPLC/Orbitrap HRMS)technique. Ultraviolet absorbers in textiles were first ultrasonically extracted using methanol as the extraction solvent. Then, the extract was concentrated and analyzed by UPLC/Orbitrap HRMS. The quantitative analysis was carried out by the peak area in extracted chromatogram, and the concentration of each analyte was calibrated by the external standard method. The chromatographic separation of nineteen ultraviolet absorbers was carried out on a Hypersil Gold column(100 mm×2.1 mm, 1.9 μm)by gradient elution of methanol and water. The mass spectrometry analysis was carried out by Orbitrap HRMS in ESI+ and ESI- modes. Full-scan experiment was carried out in the range for m/z from 100 to 700. The screening and qualitative analysis were carried out by the retention time and the accurate mass of quasi-molecular ion and nineteen ultraviolet absorbers were routinely detected with mass accuracy errors below 2×10-6. The confirmation analysis for target compounds was performed with qualitative fragments obtained by data-dependent scan mode. The limits of quantification varied from 0.01 to 0.50 μg/kg. The blank samples were spiked at three levels, and the average spiked recoveries changed from 82.35% to 94.58% with the relative standard deviation(RSD)-changing from 3.37% to 9.98%. The proposed method was applied in the rapid screening of ultraviolet absorbers in textiles available commercially and UV-327 was detected in one sample.

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