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《天津医科大学学报》[ISSN:1006-8147/CN:12-1259/R]

卷:

25卷

期数:

2019年04期

页码:

320-323328

栏目:

基础医学

出版日期:

2019-07-20

文章信息/Info

Title:

Determination of acetaldehyde in drug intermediates 2-methylimidazole by GC direct injection

文章编号:

1006-8147(2019)04-0320-04

作者:

翁秀芳¹; 董卫莉¹; 张慕军²

（1. 天津医科大学药学院药物化学教研室，天津市临床药物关键技术重点实验室，天津300070；2. 天津药物研究院原料药研究中心，天津300193）

Author(s):

WENG Xiu-fang¹;  DONG Wei-li¹;  ZHANG Mu-jun²

(1. Department of Medical Chemistry, School of Pharmacy, Tianjin Medical University, Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnosthcs(Theranostics), Tianjin 300070, China; 2 Active Pharmaceutical Ingredient Research Center, Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China)

关键词:

气相色谱法; 液体进样; 2-甲基咪唑; 乙醛; 残留量测定

Keywords:

GC (Gas chromatography);  direct injection; 2-methylimidazole; acetaldehyde; residue

分类号:

R961

DOI:

-

文献标志码:

A

摘要:

目的：建立药物中间体2-甲基咪唑中乙醛残留量的测定方法。方法：采用气相色谱法，液体进样，以Agilent DB-624（75 m × 530 μm × 3 μm）为分析柱，FID检测器；恒温：50 ℃，保持5.5 min；N2流量为6 mL·min-1；后运行：温度为240 ℃，保持10.5 min, 流量为8 mL·min-1。采用外标法。结果：液体进样可以避免高温条件下的基质效应对乙醛测定的影响，乙醛在1.36~ 188.96 μm·mL-1内线性关系良好，R2=0.999 9，方法的回收率在99.74％~102.87％且RSD（n=9）=1.19％，最低检出限为0.55 μm·mL-1。结论：气相液体进样法操作简单、专属性强、重现性强、灵敏度高，可以用于乙醛残留量的检测。

Abstract:

Objective: To establish a GC method for determination of acetaldehyde in drug intermediates 2-methylimidazole. Methods: GC direct injection was performed on Aglilent DB-624(75 m × 530 μm × 3 μm) with FID detector. The column temperature was controlled at 50 ℃, maintained for 5.5 min at the flow rate of N2 of 6 mL·min-1. The postrun temperature was controlled at 240 ℃, maintained for 10.5 min at the flow rate of N2 of 8 mL·min-1. External reference method was applied to analyze data. Results: Under the chromatographic condition mentioned above, the influence of matrix effect was ignored. The calibrated linear curve of acetaldehyde was in between the rang of 1.36~188.96 μm·mL-1 with R2 = 0.999 9. The average recovery of acetaldehyde was between 99.74％ and 102.87％ with RSD(n=9) =1.19％, 0.55 μm·mL-1 was lower limit of detection for this method. Conclusion: The determination of acetaldehyde may be solved by GC indirect injection, indicating the good specificity, high reproducibility and high sensitivity.

参考文献/References:

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备注/Memo

备注/Memo:

作者简介 翁秀芳（1993-），女，硕士在读，研究方向：药学;通信作者： 董卫莉，E-mail: dongweili@tmu.edu.cn，张慕军，E-mail: 20072328@qq.com。

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更新日期/Last Update: 2019-08-28