论文部分内容阅读
目的建立药用辅料醋酸中残留乙醛的测定方法。方法醋酸用水稀释一倍后用等量的碱中和为盐溶液,立即密封后,采用顶空气相色谱法测定,以HP-INNOWAX石英毛细管柱(30 m×0.32 mm,0.5μm)为分析柱,FID检测器;程序升温:35℃维持5 min,然后以30℃·min-1升温至120℃,保持2 min;N2流速为3.0 mL·min-1;顶空进样:80℃平衡30 min。结果醋酸的稀释避免了大量放热对测定的影响,中和生成的盐溶液提高了方法检测灵敏度,乙醛在10.73~107.3-g·mL-1(r=0.999 8)内线性关系良好,方法回收率为95.8%(n=9,RSD=5.0%),最低检出限为2.5-g。结论用简单的顶空气相色谱法,解决了醋酸中痕量乙醛残留的测定问题,为其国家标准的修订奠定了基础。
Objective To establish a method for the determination of residual acetaldehyde in pharmaceutical excipients. Methods Acetic acid was diluted twice with water and neutralized with an equal amount of base to form a salt solution. Immediately after sealing, the sample was analyzed by headspace gas chromatography (HP-INNOWAX) (30 m × 0.32 mm, 0.5 μm) , FID detector; program temperature: 35 ℃ for 5 min, then 30 ℃ · min-1 to 120 ℃, hold 2 min; N2 flow rate 3.0 mL · min-1; min. As a result, the acetic acid dilution avoided the influence of a large amount of exotherm on the determination. Neutralization of the generated salt solution increased the sensitivity of the method, and the linear relationship was good between 10.73 and 107.3-g · mL-1 acetaldehyde (r = 0.999 8) The recovery was 95.8% (n = 9, RSD = 5.0%) with a minimum detectable limit of 2.5-g. Conclusion The determination of trace acetaldehyde residues in acetic acid was solved by simple headspace gas chromatography, which laid the foundation for the revision of its national standards.