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,2021,42(9):177-183.
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,2021,42(9):177-183. |
| GC-MS法测定药用复合包装袋中异氰酸酯 |
| Determination of Isocyanates in Medicinal Composite Packaging Bag by Gas Chromatography-Mass Spectrometry |
| 投稿时间：2020-08-12 |
| DOI：10.19554/j.cnki.1001-3563.2021.09.024 |
| 中文关键词: 气相色谱-质谱法 药用复合包装袋 异氰酸酯 药品包装材料 |
| 英文关键词: gas chromatography-mass spectrometry medicinal composite packaging bag isocyanate drug package materials |
| 基金项目: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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| 中文摘要: |
| 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。 |
| 英文摘要: |
| 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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