纺织学报 ›› 2022, Vol. 43 ›› Issue (12): 125-130.doi: 10.13475/j.fzxb.20211107106

• 染整与化学品 • 上一篇    下一篇

纺织品中喹啉含量的快速测定

尹喆1,2, 赵海浪2(), 徐红1, 毛志平1, 谭玉静2   

  1. 1.东华大学 生态纺织品教育部重点实验室, 上海 201620
    2.上海市质量监督检验技术研究院, 上海 200040
  • 收稿日期:2021-11-16 修回日期:2022-09-14 出版日期:2022-12-15 发布日期:2023-01-06
  • 通讯作者: 赵海浪
  • 作者简介:尹喆(1997—),女,硕士生。主要研究方向为生态纺织品中有害物质检测。
  • 基金资助:
    上海市科技创新行动计划项目(20142202400)

Rapid determination of quinoline in textiles

YIN Zhe1,2, ZHAO Hailang2(), XU Hong1, MAO Zhiping1, TAN Yujing2   

  1. 1. Key Laboratory of Science & Technology of Eco-Textile, Ministry of Education, Donghua University, Shanghai 201620, China
    2. Shanghai Institute of Quality Inspection and Technical Research, Shanghai 200040, China
  • Received:2021-11-16 Revised:2022-09-14 Published:2022-12-15 Online:2023-01-06
  • Contact: ZHAO Hailang

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摘要：

为解决现有纺织品中喹啉化学提取法样品提取时间长、有机试剂用量大的问题,建立了热裂解/热脱附-气相色谱-质谱(Py/TD-GC-MS)法快速测定纺织品中喹啉的分析方法。该方法所测样品无需处理,直接在热裂解/热脱附装置中热脱附出喹啉,再进入气相色谱-质谱联用仪进行定性和定量测定。针对喹啉标准溶液中喹啉在等待分析过程中挥发的问题,加入了聚氯乙烯(PVC)作为喹啉的吸附剂,提高喹啉标准溶液分析的准确性;确定了热脱附条件:温度为240 ℃,时间为6 s,升温速率为50 ℃/min,接口温度为300 ℃。结果表明,该方法在线性范围 10~1 000 mg/kg内,相关系数为0.994,方法检出限为3.520 mg/kg,定量限为11.760 mg/kg,加标回收率为 90.02%~102.07%, 相对标准偏差为1.27%~4.53%,适用于纺织品中喹啉的快速测定。

关键词: 纺织品, 喹啉, 吸附剂, 热脱附-气相色谱-质谱分析, 快速测定, 聚氯乙烯

Abstract:

In order to reduce the extraction time from small amount of organic reagent, a rapid analytical method for the determination of quinoline in textiles by pyrolysis/thermal desorption-gas chromatography-mass spectrometry(Py/TD-GC-MS) was established. This method requires no sample processing, and the quinoline is thermally desorbed directly in the pyrolysis/thermal desorption device before entering the GC-MS for qualitative and quantitative determination. To solve the problem of quinoline volatilization before and during the analysis process, polyvinyl chloride(PVC) was added as the adsorbent of quinoline to improve the accuracy of quinoline standard solution analysis. The thermal desorption temperature was 240 ℃, the thermal desorption time was 6 s, the heating rate was 50 ℃/min and the interface temperature was 300 ℃. The results show that the linear range of the method was 10-1 000 mg/kg, the correlation coefficient was 0.994, the limit of detection was 3.520 mg/kg, the limit of quantification was 11.760 mg/kg, the spiked recoveries were 90.02%-102.07%, and the relative standard deviation was 1.27%-4.53%. All these suggest that this method is suitable for rapid determination of quinoline in textiles.

Key words: textile, quinoline, adsorbent, thermal desorption-gas chromatography-mass spectrometry, rapid determination method, polyvinyl chloride

中图分类号: 

  • O657.63

图1

等待时间对喹啉质谱响应强度的影响"

图2

PVC溶液质量浓度对喹啉质谱响应强度的影响"

图3

PVC溶液和喹啉标准溶液B的EGA-MS选择离子图"

图4

热脱附温度对喹啉质谱响应强度的影响"

图5

热脱附时间对喹啉质谱响应强度的影响"

图6

升温速率对喹啉质谱响应强度的影响"

图7

接口温度对喹啉质谱响应强度的影响"

图8

喹啉标准曲线的线性关系"

表1

喹啉的加标回收率及重现性"

纺织面料 加标量/(mg·kg-1) 平均加标回收率/% RSD/%
棉 10 91.79 4.22
200 96.77 1.89
1 000 102.07 3.44
羊毛 10 94.51 4.53
200 97.84 3.33
1 000 101.31 1.27
涤纶 10 90.75 4.25
200 94.92 1.54
1 000 98.59 1.71
锦纶 10 90.02 3.93
200 93.13 1.48
1 000 97.49 1.63

表2

化学提取检测法与Py/TD-GC-MS法比较"

检测方法 样品处理
有机试剂		 样品处理
时间/min		 喹啉含量/(mg·kg-1)
橙色纱线 黑色纱线
化学提取检测法 15 mL甲醇 30 69.73 60.33
Py/TD-GC-MS法 - 5 91.63 79.04
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