安全监测

气相色谱-质谱法测定药用复合膜中16种光引发剂的残留量*

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  • 重庆市食品药品检验检测研究院 国家药品监督管理局麻醉精神药品质量监测重点实验室,重庆 401121
Tel:(023)86072759;E-mail:wuhongyang@cqifdc.org.cn

收稿日期: 2023-08-14

  网络出版日期: 2024-06-20

基金资助

* 重庆市绩效引导专项项目(CQIFDC-YJKT-2021-14)和2023年重庆市药品补充检验方法项目资助

Determination of 16 photoinitiator residuces in medicinal composite membranes with gas chromatography-mass spectrometry*

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  • Chongqing Institute for Food and Drug Control, NMPA Key Laboratory for Quality Monitoring of Narcotic Drugs and Psychotropic Substances, Chongqing 401121, China

Received date: 2023-08-14

  Online published: 2024-06-20

摘要

目的:建立气相色谱-质谱法同时测定药用复合膜中二苯甲酮、4-甲基二苯甲酮等16种光引发剂的残留量。方法:样品经乙酸乙酯超声提取后,采用TR-5MS气相色谱柱,程序升温;质谱检测器:电子轰击源,正离子模式,选择反应监测模式下进行分析,内标法定量。结果:16种光引发剂在0.05~2.0 μg·mL-1范围内线性关系良好,r均>0.997,检测限均为0.03 μg·mL-1,平均回收率(n=6)在81.3%~94.0%,RSD为2.1%~6.2%。10批次药用复合膜中光引发剂4-ITX检出率为30%,最高含量为0.02 μg·cm-2结论:该方法前处理简单,灵敏度高,结果准确,可用于药用复合膜中多种光引发剂残留量的同时测定。

本文引用格式

吴红洋 . 气相色谱-质谱法测定药用复合膜中16种光引发剂的残留量*[J]. 药物分析杂志, 2024 , 44(5) : 851 -858 . DOI: 10.16155/j.0254-1793.2024.05.13

Abstract

Objective: To establish a gas chromatography-mass spectrometry (GC-MS) method for the determination of 16 photoinitiator residuce levels in medicinal composite membranes, including benzophenone (BP) and 4-methylbenzophenone (4-MBP). Methods: The samples were extracted by ethylacetate, separated with TR-5MS column. The mass spectrum was analyzed with EI ionization, positive ion mode and selective reaction monitoring (SRM) mode and quantified with internal standard method. Results: The 16 kinds of photoinitiators had good linear relationships in the range of 0.05-2.0 μg·mL-1, and the correlation coefficients (r) were more than 0.997. The limits of detection (LODs) were 0.03 μg·mL-1. The average recoveries were (n=6) ranged from 81.3% to 94.0%, with RSDs of 2.1%-6.2%. The detection rate of 4-Isopropylthioxanthone (4-ITX) in the medicinal composite membranes was 30%, and the highest content was 0.02 μg·cm-2. Conclusion: The method is accurate with high sensitivity and simple pretreatment, which can be used for the detecting the kinds of photoinitiators in medicinal composite membranes.

参考文献

[1] 武青青,沈虎峻,邓明森.可见光引发剂研究进展[J]. 涂料工业,2020,50(8):71
WU QQ, SHEN HJ, DENG MS. The research progress in visible light photoinitiator[J]. Paint Coat Ind, 2020, 50(8):71
[2] 刘珊珊,柯玮,范子彦,等.食品接触材料中光引发剂残留及其迁移规律研究进展[J]. 中国食品卫生杂志,2014,26(5):507
LIU SS,KE W, FAN ZY, et al. Research progress in residue analysis of photoinitiators in food contact materials and migration in food matrices[J]. Chin J Food Hyg, 2014, 26(5):507
[3] VAN-DEN HK, VANDE-VELDE S, EVRARD C, et al. Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)[J]. Food Addit Contam, 2014, 31(4):767
[4] 赵镭,袁琳嫣,韩陈.气相色谱-质谱法测定食品包装行业用UV油墨中11种光引发剂的含量[J]. 食品安全质量检测学报,2020,11(7):2162
ZHAO L, YUAN LY, HAN C. Determination of 11 photoinitiators in UK ink for food packaging industry by gas chromatography-mass spectrometry[J]. J Food Saf Food Qual, 2020, 11(7):2162
[5] RHODES MC, BUCHER JR, PECKHAM JC, et al. Carcinogenesis studies of benzophenone in rats and mice[J]. Food Chem Toxicol, 2007, 45(5):843
[6] Council of Europe. Policy statement concerning paper and board materials and articles intended to come into contact with foodstuffs[EB/OL]. (2009-12-02) [2023-07-13]. https://rm.coe.int/09000016804e4794
[7] European Commission Health and Consumers Directorate-General. Conclusions of standing committee on the food chain and animal health section toxicological safety conclusions of the meeting [EB/OL]. (2009-03-06)[2023-07-13]. https://ec.europa.eu/commission/presscorner/detail/en/memo_05_154
[8] 倪勇.提高食品包装UV油墨的标准以引领高质量发展[C]//第十八届中国标准化论坛论文集. 2021:1334
NI Y. Improve food packaging UV ink standards to lead the development of high quality[C]//Proceedings of the 18th China Standardization Forum. 2021:1334
[9] GB 9685-2016食品安全国家标准. 食品接触材料及制品用添加剂使用标准[S]. 2016
GB 9685-2016 National Food Safety Standard. Standards for The Use of Additives for Food Contact Materials and Products [S]. 2016
[10] 李中皓,吴帅宾,刘珊珊,等.超高效合相色谱法快速检测纸质印刷包装材料中10种受限制光引发剂[J]. 分析化学, 2013,41(12):1817
LI ZH, WU SB, LIU SS, et al. Rapid detection of tenrestricted photoinitiators in paper-made packaging based on ultra performance convergence chromatography [J]. Chin J Anal Chem, 2013, 41(12):1817
[11] 沈康俊,赵洁,吴之中,等.高效液相色谱-串联质谱法检测食品接触材料及制品中8种二苯甲酮类物质的迁移量[J]. 分析试验室,2022,41(3):322
SHEN KJ, ZHAO J, WU ZZ, et al. Determination of the migration of 8 benzophenones in food contact materials and products by HPLC-MS/MS[J]. Chin J Anal Lab, 2022, 41(3):322
[12] 陶小美,罗小芳,胡爱生.超声萃取-超高效液相色谱-串联质谱法测定玩具涂层中2种光引发剂残留量[J]. 理化检验-化学分册,2021,57(9):776
TAO XM, LUO XF, HU AS. Determination of two photoinitiator residues in toy coatings by ultrasonic extraction-UHPLC-MS/MS[J]. Phys Test Chem Anal Part B:Chem Anal, 2021, 57(9):776
[13] 陶运来,田素润.凝胶渗透色谱-气相色谱-串联质谱法测定牛奶中的两种光引发剂[J]. 化学分析计量,2018,27(5):11
TAO YL,TIAN SR. Determination of two photoinitiators in milk by gel permeation chromatography-gas chromatography tandem mass spectrometry[J]. Chem Anal Meter, 2018, 27(5):11
[14] 王玉,李莹,李海山,等.气相色谱-质谱法同时测定环保型烟标胶印紫外光固化油墨中10种光引发剂的残留量[J]. 理化检验-化学分册,2022,58(2):161
WANG Y, LI Y, LI HS, et al. Simultaneous determination of residues of 10 photoinitiators in ultroviolet curing offset ink for eoo-friendly cigarette labels by gas chromatography-mass spectrometry[J]. Phys Test Chem Anal Part B:Chem Anal, 2022, 58(2):161
[15] 沈丹玉,袁新跃,王蕤,等.吸附剂针对性净化-气相色谱-三重四极杆串联质谱测定油茶果中55种持久性有机污染物[J]. 质谱学报,2021,42(3):314
SHEN DY, YUAN XY, WANG R, et al. Determination of 55 persistent organic pollutants in camellia fruits by adsorbents targeted purification and gas chromatography-tandem mass spectrometry[J]. J Chin Mass Spectrom Soc, 2021, 42(3):314
[16] 闫峻,冯硕,李博文,等.气相色谱-质谱法测定石油中十二种卤代烃示踪剂[J]. 质谱学报,2020,41(4):379
YAN J, FENG S, LI BW, et al. Determination of twelve halogenated hydrocarbon organic tracersin petroleum by GC/MS[J]. J Chin Mass Spectrom Soc, 2020, 41(4):379
[17] 李重九.色谱-质谱联用技术的进步与农药多残留分析方法的发展(之二)—从低分辨质谱技术的选择性谈起[J]. 质谱学报,2021,42(5):681
LI CJ.Progress of chromatography-mass spectrometry technology and development of pesticide multi-residue analysis methods(part 2)-on the selectivity of low resolution mass spectrometry[J]. J Chin Mass Spectrom Soc, 2021, 42(5):681
[18] 李莎,武静文,吴红洋,等.药用复合膜中2,4-二氨基甲苯的检测[J]. 药物分析杂志, 2022,42(7):1234
LI S, WU JW, WU HY, et al. Detection of 2,4-diaminotoluene in medicinal composite membranes[J]. Chin J Pharm Anal, 2022, 42(7):1234
[19] 吴泽颖,裴文艺,毕中昱,等.基于GC-MS法测定纸质包装中4种二苯甲酮类物质[J]. 包装工程,2021,42(1):109
WU ZY, PEI WY, BI ZY, et al. Determination of 4 kinds of benzophenones in paper packaging by gas chromatography-mass spectrometry[J]. Package Eng, 2021, 42(1):109
[20] 周良春,马俊辉,张晓飞,等.GC-MS法快速测定铅笔涂层中18种光引发剂[J]. 分析试验室, 2021, 40(1):95
ZHOU LC, MA JH, ZHANG XF, et al. Rapid determination of 18 photoinitiators in pencil coating by GC-MS[J]. Chin J Anal Lab, 2021, 40(1):95
[21] 吴泽颖,裴文艺,毕中昱,等.皮革制品中光引发剂含量的测定[J]. 皮革科学与工程,2021,31(1):60
WU ZY, PEI WY, BI ZY, et al. Determination of photoinitiators in leather products[J]. J Leather Sci Eng, 2021, 31(1):60
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