GC-MS法测定药用复合包装袋中异氰酸酯

张清, 邱月, 余秋玲, 龙梅, 陈豪, 张永梅

包装工程(技术栏目) ›› 2021 ›› Issue (9) : 177-183.

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包装工程(技术栏目) ›› 2021 ›› Issue (9) : 177-183. DOI: 10.19554/j.cnki.1001-3563.2021.09.024

GC-MS法测定药用复合包装袋中异氰酸酯

  • 张清, 邱月, 余秋玲, 龙梅, 陈豪, 张永梅
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Determination of Isocyanates in Medicinal Composite Packaging Bag by Gas Chromatography-Mass Spectrometry

  • ZHANG Qing, QIU Yue, YU Qiu-ling, LONG Mei, CHEN Hao, ZHANG Yong-mei
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摘要

目的 利用气相色谱-质谱(GC-MS)技术建立同时测定药用复合包装袋中8种异氰酸酯含量的方法。方法 将药用复合包装袋剪成尺寸(长×宽)不大于5 mm×5 mm的小碎片,采用二氯甲烷超声萃取40 min;萃取液经氮吹浓缩后,采用GC-MS法分析。采用TG-5MS色谱柱,将进样口温度设为200 ℃,柱温箱初温设为40 ℃,在程序升温条件下可实现8种异氰酸酯的有效分离。结果 8种异氰酸酯在质量浓度为0.02~5.0 mg/L时,线性关系良好,相关系数R2均大于0.997,检出限为0.001~0.006 mg/kg。药用复合包装袋中的异氰酸酯在低、中、高等3个浓度水平下的加标回收率为80.3%~111.7%,相对标准偏差为0.6%~5.1%。结论 该方法操作简便、灵敏度高、准确度好,可为药用复合包装袋中异氰酸酯的检测分析提供技术支持。

Abstract

A method for simultaneous determination of eight isocyanates in medicinal composite packaging bags was established by gas chromatography-mass spectrometry (GC-MS). The composite packaging bag was cut into small pieces no larger than 5 mm×5 mm, and then extracted by dichloromethane for 40 min. The extraction solution was analyzed by GC-MS after concentration by nitrogen blowing. Eight isocyanates could be separated and detected using TG-5MS column with injection temperature of 200 ℃ and initial temperature of column incubator of 40 ℃. Eight isocyanates had a good linear relationships in the range of 0.02 to 5.0 mg/L with the correlation coefficient greater than 0.997. The detection limit was in the range of 0.001~0.006 mg/kg. The recovery for accuracy at low, medium and high concentration levels was ranged from 80.3% to 111.7%, and the relative standard deviation for repeatability was between 0.6% and 5.1%. This method is simple, sensitive and accurate, which can provide technical support for the detection and analysis of isocyanate in medicinal composite packaging bag.

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张清, 邱月, 余秋玲, 龙梅, 陈豪, 张永梅. GC-MS法测定药用复合包装袋中异氰酸酯[J]. 包装工程(技术栏目). 2021(9): 177-183 https://doi.org/10.19554/j.cnki.1001-3563.2021.09.024
ZHANG Qing, QIU Yue, YU Qiu-ling, LONG Mei, CHEN Hao, ZHANG Yong-mei. Determination of Isocyanates in Medicinal Composite Packaging Bag by Gas Chromatography-Mass Spectrometry[J]. Packaging Engineering. 2021(9): 177-183 https://doi.org/10.19554/j.cnki.1001-3563.2021.09.024

基金

重庆市市场监督管理局项目(CQSJKJ2019005);重庆市计量质量检测研究院自立项目(2019(研)-09)

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