异噻唑啉酮类防腐剂标准现状及检测技术研究进展

doi:10.3969/j.issn.2097-2806.2023.10.010

摘要/Abstract

摘要：

异噻唑啉酮类防腐剂因其广谱高效和环境友好等特点，在化妆品、玩具、涂料等领域广泛应用。国内外关于异噻唑啉酮类防腐剂引起的过敏反应或接触性皮炎，甚至皮肤灼伤的报道越来越多，引发社会高度关注。关注异噻唑啉酮类防腐剂相关法规标准，选择准确高效的分析方法，对其进行安全性风险评估具有重要意义。本文总结了欧盟和中国对异噻唑啉酮类防腐剂的限量要求，以及国内目前的检测标准现状。简要概述了加速溶剂萃取法、固相萃取法、QuEchERS等前处理技术，重点综述了气相色谱法、气相色谱-质谱法、液相色谱法和液相色谱-串联质谱法等检测分析技术在异噻唑啉酮类防腐剂中的应用。最后对该类防腐剂检测方法研究的发展方向进行了展望，以期为相关研究人员和完善相关标准体系提供参考。

关键词: 异噻唑啉酮类防腐剂, 应用, 标准, 检测技术, 综述

Abstract:

Isothiazolinone preservatives are broad-spectrum, high-efficiency and environmentally friendly, which have been widely used in cosmetics, toys, coatings and other fields. However, there are more and more reports at home and abroad about allergic reactions, contact dermatitis, and even chemical skin burns caused by isothiazolinone preservatives, which has aroused concerns in society. It is of great significance to pay attention to the relevant regulations and standards of isothiazolinone preservatives and select accurate and efficient analytical methods for their safety risk assessments. Herein, a comprehensive overview on the limits of content of isothiazolinone preservatives in European Union and China was made, as well as the domestic situation of detection standards. The pretreatment techniques, including accelerated solvent extraction, solid-phase extraction, and QuEChERS, were briefly reviewed. The applications of gas chromatography, gas chromatography-mass spectrometry, liquid chromatography, and liquid chromatography-tandem mass spectrometry for isothiazolinone preservatives were reviewed. Finally, the development direction of detection techniques for isothiazolinone preservatives in different products was prospected, in order to provide reference to related researchers and improve the relevant standard system.

Key words: isothiazolinone preservative, application, standard, detection technique, review

中图分类号:

TQ658

何小玲, 马艳, 邓星, 陆嘉莉, 吴荣荣, 龙梅. 异噻唑啉酮类防腐剂标准现状及检测技术研究进展[J]. 日用化学工业（中英文）, 2023, 53(10): 1186-1193.

He Xiaoling, Ma Yan, Deng Xing, Lu Jiali, Wu Rongrong, Long Mei. Current status of standards and research progress of detection methods of isothiazolinone preservatives[J]. China Surfactant Detergent & Cosmetics, 2023, 53(10): 1186-1193.

图/表 3

表1

表2

表3

部分代表性检测方法的比较"

产品	分析物质	前处理技术	分析技术	色谱柱	检出限	回收率/%	精密度/%	参考文献
化妆品	MIT、CMIT	LLE	HPLC-DAD	Apollo Phenyl column	0.03, 0.090 mg/mL	86.5~101.8	2.5~5.2	[23]
烟用香精香料	MIT、CMIT	OE	HPLC-MS/MS	Agilent ZORBAX 300SB-C8	3.2, 3.6 μg/L	77.1~95.0	1.0~5.0	[24]
水性涂料	MIT、CMIT、BIT、OIT、DCOIT	UE	HPLC-MS/MS	Agilent Zorbax Eclipse Plus C18	0.001 3~0.420 0 mg/kg	86.73~93.6	2.3~5.8	[25]
纺织品	OIT等	ASE	HPLC-DAD	Agilent 1200 C18	LOQ：0.16 mg/kg	94.9~97.3	7.3~8.4	[26]
纺织品	OIT等	ASE	GC-MS	DB-1MS	LOQ：0.09 mg/kg	96.7~97.9	5.4~6.3	[26]
皮革及制品	MIT、CMIT、BIT、BBIT、MBIT、OIT、DCOIT	SPE	GC-MS	RXi-5MS	OIT, MBIT, BBIT: 0.05 mg/kg；MIT, CMIT, BIT, DCOIT：0.10 mg/kg	80.21~95.87	1.26~4.85	[27]
烟用纸	MIT、CMIT	DSPE	GC-MS	HP-5MS	0.007，0.012 μg/mL	92.59~107.62	1.32~7.99	[28]
个人护理用品	MIT、CMIT等	UE	HPLC-DAD-FLD	KromaPhase 5μm C18	11，55 μg/L	80~113	0.9, 2.2	[40]
保健品	MIT、CMIT等	UE	GC-MS	DB-624UI	0.002 mg/L	96.2~107.6	0.4~5.3	[41]
家用液体洗涤剂	MIT、CMIT、BIT、DCOIT	UE	UPLC- MS/MS	Waters ACQUITY UPLC HSS T3 C18	0.05 mg/kg	81.2~103.2	2.23~4.52	[42]
木材及木制品	MIT、CMIT、BIT	UE	HPLC-MS/MS	Eclipse Plus C18	0.04，0.13，0.12 mg/kg	85~111	0.93~8.20	[43]
湿纸巾	MIT、CMIT、BIT、OIT、DCOIT	QuEChERS	UPLC-MS/MS	Waters ACQUITY UPLC HSS T3 C18	LOQ：0.005 mg/kg	91.1~103.5	2.11~3.27	[44]
水基胶	MIT、CMIT	TP-HF-LPME	HPLC-DAD	Waters Prontosil 120-5-C18 AQ	0.037~0.147 μg/g	102~103	1.2~11.7	[45]
水基胶	MIT、CMIT	TP-HF-LPME	UPLC-Q-TOF-MS	Waters UPLCBEH C18	0.004~0.007 μg/g		2.4~4.1	[45]
再造烟叶	MIT、CMIT	QuEChERS	HPLC-MS/MS	Agilent ZORBAX 300SB-C8	LOQ：2.5，2.8 μg/L	90.2~98.3	1.0~5.0	[46]
饲料	MIT、CMIT、BIT	SPE	HPLC-MS/MS	Eclipse Plus C18	0.010~0.015 mg/L	75.8~102	1.63~5.75	[47]
海水	BIT、OIT、DCOIT等	SPE	HPLC-DAD	Agilent Eclipse XDB-C18	1.7×10^-6，3.6×10^-7，2.5×10^-7mol/L	96~110	<4	[48]

表3

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