超高效液相色谱法测定烟用水基胶中3种异噻唑啉酮杀菌剂
UHPLC Determination of 3 Isothiazolinone Bactericides in Water-Based Adhesive for Cigarettes
摘 要
采用超声提取-超高效液相色谱法同时测定烟用水基胶中3种异噻唑啉酮类化合物的含量。样品0.300 0 g经20 mL甲醇（1+1）溶液超声提取30 min后，提取液在Waters ACQUITY UPLC HSS T3色谱柱上分离，以水-乙腈混合液为流动相进行梯度洗脱，采用二极管阵列检测器进行检测，检测波长为275 nm和318 nm。3种异噻唑啉酮类化合物的质量浓度在一定范围内与其峰面积呈线性关系，检出限（3S/N）在0.005~0.01 mg·L-1之间，测定下限（10S/N）在0.015~0.03 mg·L-1之间。加标回收率在92.2%~100%之间，测定值的相对标准偏差（n=6）在1.2%~6.0%之间。
超声提取
异噻唑啉酮
烟用水基胶
UHPLC
Ultrasonic extraction
Isothiazolinone
Water-based adhesive for cigarett
Abstract
UHPLC combined with ultrasonic extraction was applied to the simultaneous determination of 3 isothiazolinones in water-based adhesive for cigarettes. The sample (0.300 0 g) was extracted by ultrasonic with 20 mL of methanol solution (1+1) for 30 min. The extract was separated on a Waters ACQUITY UPLC HSS T3 chromatographic column with the mixture of water and acetonitrile as mobile phase in gradient elution. Anlytes were detected by diode array detector at the wavelength of 275 nm and 318 nm. Linear relationships were found between values of peak area and mass concentration of the 3 isothiazolinones in definite ranges, with detection limits (3S/N) in the range of 0.005-0.01 mg·L-1, and lower limits of determination (10S/N) in the range of 0.015-0.03 mg·L-1. Recoveries obtained by standard addition method were in the range of 92.2%-100% and RSDs (n=6) were in the range of 1.2%-6.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201704013
所属栏目 工作简报
基金项目 贵州中烟工业有限责任公司科技项目（201316）
收稿日期 2016/4/11
修改稿日期
网络出版日期
作者单位点击查看
联系人作者刘剑(liuj1208@163.com)
备注姬厚伟(1978-),男,河南新乡人,工程师,硕士,主要从事烟用材料及烟草化学分析研究。
引用该论文: JI Hou-wei,DONG Rui,LIU Jian,ZHANG Li,WANG Fang,HUANG Xi-juan,PENG Qian-rong. UHPLC Determination of 3 Isothiazolinone Bactericides in Water-Based Adhesive for Cigarettes[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(4): 432～436
姬厚伟,董睿,刘剑,张丽,王芳,黄锡娟,彭黔荣. 超高效液相色谱法测定烟用水基胶中3种异噻唑啉酮杀菌剂[J]. 理化检验－化学分册, 2017, 53(4): 432～436
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参考文献
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【2】付忠叶,王庆,贾兰妮,等.异噻唑啉酮衍生物近10年的制备和应用研究进展[J].材料导报, 2012,26(s1):291-296.
【3】邬庆梅.异噻唑啉酮防腐剂——一种化妆品皮炎持续流行的病因[J].国外医学(卫生学分册), 1990(3):191-192.
【4】JERSCHOW E, HOSTYNEK J J, MAIBACH H I. Allergic contact dermatitis elicitation thresholds of potent allergens in humans[J]. Food and Chemical Toxicology, 2001,39(11):1095-1108.
【5】司新生,杨俊伟,杭磊.日化级异噻唑啉酮类杀菌防腐剂皮肤刺激实验及其机理的研究[J].应用化工, 2011,40(10):1789-1791.
【6】EN 71-9-2005 Safety of toys-Organic chemical compounds-Requirements[S].
【7】GB 9685-2008 食品容器、包装材料用添加剂使用卫生标准[S].
【8】中华人民共和国卫生部.化妆品卫生规范[S].
【9】张建枚,潘亚男,白桦.UV法测定异噻唑啉酮衍生物活性物含量[J].工业水处理, 2011,31(5):70-71.
【10】王超,张青,王星.化妆品中甲基异噻唑啉酮及其氯代物的高效液相色谱测定法[J].环境与健康杂志, 2007,24(6):449-450.
【11】赵美丽.HPLC法测定化妆品中的甲基异噻唑啉酮及其氯代物[J].江西化工, 2013(4):188-195.
【12】林芳,毛树禄,陈斌,等.皮革中异噻唑啉酮防霉剂的检测方法[J].中国皮革, 2011,40(7):5-10.
【13】刘奋,戴京晶,梁伟,等.气相色谱法测定化妆品防腐剂凯松[J].现代预防医学, 2004,31(6):872-873.
【14】NAKASHIMA H, MATSUNAGA I, MIYANO N, et al. Determination of antimicrobial agents in non-formalin adhesives for wallpaper[J]. Journal of Health Science, 2000,46(6):447-454.
【15】RAFOTH A, GABRIEL S, SACHER F, et al. Analysis of isothiazolinones in environmental waters by gas chromatography-mass spectrometry[J]. Journal of Chromatography A, 2007,1164(1/2):74-81.
【16】LIN Q B, WANG T J, SONG H, et al. Analysis of isothiazolinone biocides in paper for food packaging by ultra-high-performance liquid chromatography-tandem mass spectrometry[J]. Food Additives and Contaminants Part A, 2010,27(12):1775-1781.
【17】BESTER K, LAMANI X. Determination of biocides as well as some biocide metabolites from facade run-off waters by solid phase extraction and high performance liquid chromatographic separation and tandem mass spectrometry detection[J]. Journal of Chromatography A, 2010,1217(32):5204-5214.
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【21】ROSERO-MOREANO M, CANELLAS E, NERIN C. Three-phase hollow-fiber liquid-phase microextraction combined with HPLC-UV for the determination of isothiazolinone biocides in adhesives used for food packaging materials[J]. J Sep Sci, 2014,37(3):272-280.
【22】周晓,李小兰,陈志燕,等.高效液相色谱法测定水基胶黏剂中3种异噻唑啉酮类杀菌剂[J].色谱, 2015,33(1):75-79.
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