色谱

色谱 ›› 2018, Vol. 36 ›› Issue (7): 670-677.DOI: 10.3724/SP.J.1123.2018.01043

• 研究论文 • 上一篇    下一篇

超高效液相色谱法同时测定纺织品中18种荧光增白剂

汤娟, 周佳, 钱凯, 丁友超, 程月, 齐琰   

  1. 江苏出入境检验检疫局工业产品检测中心, 江苏 南京 210019
  • 收稿日期:2018-01-25 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 丁友超,E-mail:dingyc@jsciq.gov.cn
  • 基金资助:

    国家质检总局科技计划项目（2017IK009）.

Simultaneous determination of 18 fluorescent whitening agents in textiles by ultra performance liquid chromatography

TANG Juan, ZHOU Jia, QIAN Kai, DING Youchao, CHENG Yue, QI Yan   

  1. Inspection Center of Industry Products, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210019, China
  • Received:2018-01-25 Online:2018-07-08 Published:2014-06-03
  • Supported by:

    Science and Technology Planning Project of General Administration of Quality Supervision, Inspection and Quarantine(No. 2017IK009).

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摘要：

建立了同时测定纺织品中18种荧光增白剂（FWAs）的超高效液相色谱-荧光检测（UPLC-FLR）法。试样由三氯甲烷-乙醇（6：4，v/v）超声提取，以ACQUITY UPLC HSS T3柱（100 mm×2.1 mm，1.8 μm）为分离色谱柱进行分析，以5 mmol/L乙酸铵水溶液和甲醇为流动相，梯度洗脱，流速为0.4 mL/min，荧光激发波长为350 nm，发射波长为430 nm，外标法定量。18种FWAs在各自范围内呈良好的线性关系，相关系数（R2）均≥ 0.9992；方法的定量限（LOQs，S/N=10）为0.002~0.1 mg/L。样品的平均加标回收率为88.3%~104.5%，相对标准偏差（RSD）为2.0%~5.5%（n=6）。该方法灵敏度高，精密度好，准确度高，适用于各种纺织品中FWAs的测定。

关键词: 超高效液相色谱, 纺织品, 荧光检测, 荧光增白剂

Abstract:

A method was developed for the simultaneous determination of 18 fluorescent white-ning agents (FWAs) in textiles by ultra performance liquid chromatography with fluorescence detection (UPLC-FLR). The sample was extracted with chloroform-ethanol (6:4, v/v). The separation was performed on an ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with gradient elution. Methanol-water (containing 5 mmol/L ammonium acetate) was used as the mobile phase with a flow rate of 0.4 mL/min. The fluorescence detector was used at 350 nm excitation wavelength and 430 nm emission wavelength. External standard method was used for the quantitative determination. The calibration curves showed good linearity in respective ranges for the 18 FWAs with correlation coefficients (R2) no less than 0.9992. The limits of quantifications (LOQs, S/N=10) were in the range of 0.002-0.1 mg/L. The average recoveries of the 18 FWAs ranged from 88.3% to 104.5% at the different spiked levels with the relative standard deviations (RSDs) of 2.0%-5.5% (n=6). The method has high sensitivity, good precision and accuracy, and is applicable to the determination of all kinds of textiles.

Key words: fluorescence detection(FLR), fluorescent whitening agents(FWAs), textiles, ultra performance liquid chromatography(UPLC)

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