理化检验-化学分册2024,Vol.60Issue(8) :837-840.DOI:10.11973/lhjy-hx220686

顶空-气相色谱法测定医用口罩中4种挥发性化学物质的残留量

Determination of Residues of 4 Volatile Chemicals in Medical Masks by Gas Chromatography with Headspace

郭锦材 谢辉 肖体敢 陈钦钦 陈同强
理化检验-化学分册2024,Vol.60Issue(8) :837-840.DOI:10.11973/lhjy-hx220686

顶空-气相色谱法测定医用口罩中4种挥发性化学物质的残留量

Determination of Residues of 4 Volatile Chemicals in Medical Masks by Gas Chromatography with Headspace

郭锦材 1谢辉 2肖体敢 3陈钦钦 3陈同强4
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作者信息

  • 1. 长沙市口腔医院,长沙 410006;湖南中医药大学口腔医学院,长沙 410006;湖南中医药大学药学院,长沙 410208
  • 2. 长沙市口腔医院,长沙 410006
  • 3. 怀化市妇幼保健院,怀化 418000
  • 4. 湖南省产商品质量检验研究院,长沙 410007
  • 折叠

摘要

通过优化色谱柱、分流比、浸提液体积、平衡时间、平衡温度等条件,提出了采用顶空-气相色谱法同时测定医用口罩中4种挥发性化学物质(甲醛、环氧乙烷、环氧丙烷、2-氯乙醇)的残留量的方法.将医用口罩裁剪成5mm×5mm的碎片.分取0.5g样品置于20mL顶空瓶中,加入5mL水(浸提液),将样品完全浸没后密封,在平衡温度80 ℃、平衡时间30 min、分流比5∶1条件下采用顶空-气相色谱仪分析.固定相选择CD-624毛细管色谱柱,在程序升温条件下用氢火焰离子化检测器(FID)检测.结果表明,4种挥发性化学物质的质量在0.10~1.0μg内和峰面积呈线性关系,检出限(3S/N)为0.05~0.1 mg·kg-1.按照标准加入法进行回收试验,回收率为84.3%~92.5%,测定值的相对标准偏差(n=6)均低于10%.方法用于市售不同品牌医用口罩的分析,均未检出4种挥发性化学物质.

Abstract

The method was proposed to simultaneously determine residues of 4 volatile chemicals(formaldehyde,ethylene oxide,propylene oxide,and 2-chloroethanol)in medical masks by gas chromatography with headspace after optimizing the chromatographic column,split ratio,extraction volume,equilibrium time,and equilibrium temperature.The medical mask was cut into fragments with the size of 5 mm×5 mm.An aliquot(0.5 g)of the sample was placed into a 20 mL-headspace bottle,and 5 mL of water(extraction solution)was added to completely immerse the sample.After sealing,the mixture was analyzed by gas chromatography with headspace under conditions of equilibrium temperature of 80 ℃,equilibrium time of 30 min,and split ratio of 5∶1.CD-624 capillary chromatographic column was adopted as the stationary phase,and targets was detected by the hydrogen flame ionization detector(FID)under programmed heating conditions.It was shown that linear relationships between values of the mass and the peak area of the 4 volatile chemicals were kept in the range of 0.10-1.0 μg,with detection limits(3S/N)in the range of 0.05-0.1 mg·kg-1.Test for recovery was made according to the standard addition method,giving recoveries in the range of 84.3%-92.5%,with RSDs(n=6)of the determined values below 10%.The proposed method was applied to the analysis of medical masks with different brands on the market,but 4 volatile chemicals were not detected.

关键词

顶空/气相色谱法/医用口罩/挥发性化学物质/残留量

Key words

headspace/gas chromatography/medical mask/volatile chemical/residue

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基金项目

湖南省自然科学基金(2024JJ9532)

湖南省卫生健康委科研计划项目(202313048136)

湖南省中医药科研课题(B2023048)

湖南中医药大学校院联合基金(2022XYLH134)

出版年

2024
理化检验-化学分册
上海材料研究所

理化检验-化学分册

CSTPCDCSCD北大核心
影响因子:0.647
ISSN:1001-4020
参考文献量11
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