气相色谱法测定硬脂酸中的脂肪酸组分

肖江,帅海涛,陈凡,黄致远,王向峰,帅放文

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主办:上海医药工业研究院
   中国药学会
   中国化学制药工业协会
ISSN 1001-8255   CN 31-1243/R   ZYGZEA
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中国医药工业杂志 ›› 2022, Vol. 53 ›› Issue (01) : 108-112. DOI: 10.16522/j.cnki.cjph.2022.01.012
研究论文 Paper

气相色谱法测定硬脂酸中的脂肪酸组分

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Determination of Fatty Acid Composition in Stearic Acid by GC

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摘要

建立了气相色谱法测定硬脂酸中脂肪酸的组成。检测前先采用甲酯化的方法,将硬脂酸中的脂肪酸转化为脂肪酸甲酯。色谱柱为DB-FFAP 毛细管柱(30 m×0.32 mm×0.5 μm),程序升温,起始温度为70 ℃,保持2 min,再以5 ℃ /min 的速率升温至240 ℃,保持24 min。进样口温度为220 ℃,氢火焰离子化检测器温度为260 ℃,分流比为10 ∶ 1。采用峰面积归一化法计算各脂肪酸甲酯含量。结果显示,所考察的16 个脂肪酸甲酯峰均可有效分离,各组分在1 ~ 100 μg/ml 内线性关系良好,精密度和稳定性均良好,各脂肪酸的检出限均低于3.4 μg/g。此外,对国内外7 个厂家的25 批样品进行了检测,均符合现行标准规定。

Abstract

A gas chromatography method was established to determine the composition of fatty acids in stearic acid. Before detection, the methyl esterification reaction was conducted to convert the fatty acids in stearic acid into fatty acid methyl esters. The DB-FFAP capillary column(30 m×0.32 mm×0.5 μm) was used. The initial column temperature was set at 70 ℃ for two minutes, followed by incraesing to the final temperature of 240 ℃ for twenty-four minutes with a rate of 5 ℃/min. The temperature of the injection port was 220 ℃, the temperature of the flame ionization detector was 260 ℃, and the split ratio was 10∶1. The peak area normalization method was used to calculate the content of each fatty acid methyl ester. The results showed that all peaks of the sixteen fatty acid methyl ester could be effectively separated. It was linear for all of them in the range of 1 - 100 μg/ml. The precision and stability were good, and the detection limit of each fatty acid was lower than 3.4 μg/g. In addition, twenty-five batches of stearic acid samples from seven domestic and foreign manufacturers were tested, and they all met the current standards.

关键词

硬脂酸 / 脂肪酸组成 / 气相色谱 / 药用辅料

Key words

stearic acid / fatty acid composition / GC / pharmaceutical excipient

引用本文

导出引用
肖江,帅海涛,陈凡,黄致远,王向峰,帅放文. 气相色谱法测定硬脂酸中的脂肪酸组分. 中国医药工业杂志. 2022, 53(01): 108-112 https://doi.org/10.16522/j.cnki.cjph.2022.01.012
XIAO Jiang, SHUAI Haitao, CHEN Fan, HUANG Zhiyuan, WANG Xiangfeng, SHUAI Fangwen. Determination of Fatty Acid Composition in Stearic Acid by GC. Chinese Journal of Pharmaceuticals. 2022, 53(01): 108-112 https://doi.org/10.16522/j.cnki.cjph.2022.01.012

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基金

湖南省自然科学基金科药联合基金(2020JJ9004)、国家药典委员会药品标准制修订研究课题(2018Y052)

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