纺织学报 ›› 2023, Vol. 44 ›› Issue (07): 222-231.doi: 10.13475/j.fzxb.20220601702

• 综合述评 • 上一篇    下一篇

纺织品中酚类化合物的法规标准及分析技术研究进展

罗忻1, 丁友超2, 叶曦雯1, 李晓瞳1,3, 高永刚1, 牛增元1()   

  1. 1.青岛海关技术中心, 山东 青岛 266109
    2.南京海关工业产品检测中心, 江苏 南京 210001
    3.中国海洋大学 环境科学与工程学院, 山东 青岛 266100
  • 收稿日期:2022-06-07 修回日期:2023-04-21 出版日期:2023-07-15 发布日期:2023-08-10
  • 通讯作者: 牛增元(1964—),男,研究员,博士。主要研究方向为消费品化学安全检测及属性鉴定。E-mail:zyniuqd@163.com
  • 作者简介:罗忻(1981—),男,研究员,硕士。主要研究方向为污染物残留分析及风险识别。
  • 基金资助:
    国家重点研发计划项目(2016YFF0203702);海关总署科研项目(2019HK070)

Advances in regulations/standards and analytical methods of phenolic compounds in textiles

LUO Xin1, DING Youchao2, YE Xiwen1, LI Xiaotong1,3, GAO Yonggang1, NIU Zengyuan1()   

  1. 1. Technology Center of Qingdao Customs, Qingdao, Shandong 266109, China
    2. Nanjing Customs District Industrial Products Inspection Center, Nanjing, Jiangsu 210001, China
    3. College of Environmental Science and Engineering, Ocean University of China, Qingdao, Shandong 266100, China
  • Received:2022-06-07 Revised:2023-04-21 Published:2023-07-15 Online:2023-08-10

摘要:

纺织品在生产加工过程中会使用或接触到各种染化料助剂,并有可能残留在最终产品中,造成潜在的环境与健康危害;同时,纺织品服装的安全环保性越来越受到重视,绿色、生态纺织品的概念逐渐深入人心。为此,以酚类化合物这一大类典型环境污染物为研究对象,概述了目前国内外纺织品法规/标准的限制和要求情况,特别讨论了法规标准中烷基酚的复杂信息。同时,从样品前处理及分析测试方法2个方面,综述了纺织品中含氯苯酚、烷基酚、双酚类等酚类化合物的检测技术和检测标准进展。最后,对该领域存在的问题和研究趋势进行了初步的小结和展望,指出开发多类别残留物筛查检测技术、实施纺织品全链条化学污染物高效识别、开展与消费者安全直接相关的暴露风险评价等未来发展方向,旨在为纺织品化学安全检测和质量控制提供有益的技术参考。

关键词: 纺织品, 化学污染物, 酚类化合物, 烷基酚, 检测标准, 分析技术

Abstract:

Significance Various types of colorants, chemicals and auxiliaries used during the production and processing progresses of textiles may eventually remain in the commercial products, causing potential hazardous risks to the environment and human health. Therefore, many countries and regions have prohibited or restricted their use in textiles. Furthermore, with the development of science and technology and the improvement of living standards, more attentions have been paid to the safety and environmental protection of textile and apparel, and the concept of green and ecological textiles has gradually gained popularity. Phenolic compounds, such as alkylphenols, were widely used in the textiles, leather, resins, dyes, pesticides, papermaking and petrochemical industries as preservatives, fungicides, adhesives, antioxidants, dye intermediates and flame retardants. In recent years, because of the increasing and stricter detection standards of phenolic compounds in textiles, the existing technologies are facing new challenges.

Progress This paper firstly reviewed the requirements of related textile regulations/standards from the aspects of limited amount of compounds, limit values, recommended testing methods, and risks of different materials. Considering the complexity of alkylphenols with a large number of isomers, this paper particularly discussed the restrictions of different regulations or standards on these substances. From the perspective of the source of regulatory material information, the analysis object of relevant environmental testing standards, and the actual industrial use, this paper provided suggestions on specific testing compounds of alkyl phenols in textiles. At the same time, this study reviewed the development progress of detection technology and detection standards for phenolic compounds, including chlorophenols, alkylphenols, bisphenols in textiles in terms of sample pretreatment and analysis methods. The extraction methods, including extractant, temperature, time and other parameters were compared in detail. Based on the requirements of regulations/standards for simultaneous determination of phenolic compounds, their salts and esters, the research and shortcomings of existing docoments in this field were discussed. As for instrument analysis, various instrumental methods for simultaneous determination of multiple phenolic compounds were described based on gas chromatography, gas chromatography-mass spectrometry, liquid chromatography, and liquid chromatography-mass spectrometry.

Conclusion and Prospect With the gradual improvement of the global chemical management system, as well as the increasing environmental protection awareness of consumers and manufacturers, some problems in the analytical field become emerging. Firstly, with the increasing number of controlled substances and the increasing severity of indicators, the conventional technology usually lags behind the regulatory requirements in terms of compound coverage, method sensitivity and selectivity. The conventional idea is to passively carry out the research of detection technology after the introduction of new regulations and requirements. Secondly, multiple classes and dozens of phenolic compounds were included in the regulations or standards, and most of the existing methods are only limited for single class of compounds. Moreover, since the risk level of the product cannot be fully understood, the detection of all classes of chemicals in ecological textiles leads to the problems of high cost and high time consumption. Thirdly, the convenitional detection model for banned substances in ecological textiles is all about the analysis of target compounds, which lacks the identification and discovery of harmful chemicals that are misused and abused in the supply chain, and the risk identification of new or alternative textile chemicals. Finally, the vast majority of textile chemical safety tests are carried out in the laboratory with large chromatographic instruments or mass spectrometers, however, methods with low-cost and rapid detection are still very rare. In addition, according to the latest research reports, some scholars are conducting extensive and in-depth research in the field of human exposure risk assessment of textile chemical residues. This direction will also be a good combination and development point of chemical analysis and environmental research of ecological textiles.

Key words: textile, chemical pollutant, phenolic compound, alkylphenol, detection standard, analytical method

中图分类号: 

  • O657

图1

壬基酚(CAS,25154-52-3)结构图(来源于SciFinder数据库) 注:D1表示虚拟的连接节点,代表羟基和壬基在苯环的连接位置不固定。"

表1

纺织品中酚类化合物检测标准前处理和分析参数汇总"

检测化合物 提取
溶剂
固液比 提取方式 提取时间 色谱柱 仪器方法 测定低限/
(mg·kg-1)
回收率 标准号
4种烷基酚
(4-n-OP、
4-tert-OP、
4-n-NP、
4-NP)
甲醇 1∶10 超声波提取
(70 ℃)
60 min HP-5MS GC-MS/MS ISO 21084:
2019
ZORBAX
Eclipse
plus C18
LC-MS/MS、
LC-FLD
2种防腐剂
(邻苯基苯酚
和三氯生)
乙腈 1∶20 超声波提取
((40±5) ℃)
(60±5) min SB C18 LC-DAD、
LC-MS
EN 17134:
2019
2,3,5,6-
四氯苯酚和
五氯苯酚
碳酸钾
溶液
1∶80 超声波提取2次
(频率40 kHz)
(20+5)min DB-17 MS GC-MS 0.05 85%~
110%
GB/T
18414.1—
2006
2,3,5,6-
四氯苯酚和
五氯苯酚
丙酮 1∶20 超声波提取3次
(频率40 kHz)
每次
15 min
DB-1701 GC-ECD 0.02 90%~
110%
GB/T
18414.2—
2006
邻苯基苯酚 甲醇 1∶50 超声波提取2次
(频率40 kHz)
(20+5) min DB-17 MS
(方法1
不衍生化,
方法2
衍生化)
GC-MS 方法1∶0.1
方法2:0.05
85%~
110%
GB/T 20386—
2006
烷基酚(4-tert-
OP和4-NP)
和烷基酚
聚氧乙烯醚
甲醇 1∶30 超声波提取
((70±2) ℃)
(60±5) min C18 LC-MS OP:0.25
NP:0.5
80%~
110%
GB/T 23322—
2018
C18 LC-MS/MS AP:0.1
C18 RPLC-FLD AP:1.0
氨基 NPLC-FLD AP:1.0
HILIC HILIC-FLD AP:1.0
壬基酚、
辛基酚、
十二烷基苯酚
正己烷 1∶20 超声波提取3次
(频率50 kHz)
每次
15 min
DB-5 GC-MS OP:3
NP:30
80%~
110%
SN/T 2583—
2010
烷基酚(4-
tert-OP、4-NP)
和烷基酚
聚氧乙烯醚
甲醇 0.5∶80 超声波提取2次 每次
30 min
ZORBAX
Extend C18
HPLC-FLD OP:0.25
NP:0.5
SN/T 3255—
2012
ACQUITY
UPLC
BEH C18
LC-MS/MS OP:0.5
NP:0.25
双酚A 甲醇 0.5∶5 超声波提取
(频率40 kHz)
20 min C18 HPLC-FLD 1.0 SN/T 4424—
2016
10种含
氯苯酚
丙酮 2∶30 超声波提取2次(频率40 kHz) 每次
20 min
ZORBAX
SB C18
HPLC-
DAD
0.01 78.8%~
105.1%
SN/T 4489—
2016
19种含
氯苯酚
甲醇 1∶20 超声波提取2次
(频率40 kHz)
每次
20 min
Poroshell 120
SB C18
LC-MS 0.05 80.3%~
103.5%
SN/T 5235—
2020
27种酚
类化合物
甲醇 1∶20 超声波提取
(频率40 kHz)
30 min C18 aQ LC-HRMS 0.002~5 61%~
117%
SN/T 5341—
2021
17种酚类化
合物
氢氧化
钾溶液
1∶20 超声波提取2次
(频率40 kHz,
(70±2) ℃)
(50+10) min DB-5 MS GC-MS 1.0 80%~
110%
SN/T 5421—
2022
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