药用油脂辅料中反式脂肪酸的GC-MS法测定

Detection of Trans Fatty Acids in Fats and Oils of Pharmaceutical Excipients

建立了气相色谱-质谱法测定药用油脂辅料中的反式脂肪酸,以提高药用油脂辅料的质量标准。样品甲酯化后,气相色谱采用SP-2560弹性石英毛细管柱,进样口温度250℃,程序升温。质谱采用电子轰击(EI)离子源,以全扫描(Scan,范围m/z 40~m/z 390)模式进行定性检测,再使用单离子监测(SIM)模式以消除背景干扰进行定量,灵敏度更高。应用本法检测Fapas(Food Analysis Performance Assessment Scheme)质控样品,以验证方法可行性和准确性,结果 |z|<2。采用本法测定药用辅料级和食用级大豆油、玉米油、花生油、橄榄油等7种油样中的反式脂肪酸,结果显示,共52组分的脂肪酸甲酯完全分离。药用大豆油中反式脂肪酸的总含量较高(>2%);其次是精制玉米油,总含量大于1%;其他5种油样中总含量较少,均小于1%。结果表明,有必要对药用油脂辅料特别是大豆油中的反式脂肪酸加以控制。

A GC-MS method was established for the determination of trans fatty acids （TFAs） in fats and oils of pharmaceutical excipients to improve the quality standard of pharmaceutical excipients. After methyl esterification, the methyl fatty acid esters were separated by SP-2560 column, the injector temperature was kept at 250℃, with colunm temperature by programed heating. Mass spectrometry was carried out by electron impact （El） ion source, with the full scan （Scan, range from m/z 40 to m/z 390） mode for qualitative detection and single-ion monitoring （SIM） mode for the elimination of background interference for quantitation. A Fapas （Food Analysis Performance Assessment Scheme） quality control sample was tested to verify the feasibility and accuracy of this method, and the result showed that ｜z｜〈2. TFAs in seven different fats and oils both of pharmaceutical excipients and food grades, including soybean oil, com oil, peanut oil, olive oil, etc., were determined by GC-MS. Methyl esters of fifty-two fatty acid could be well separated under the experiment conditions. The total content of TFAs in the soybean oil for pharmaceutical use was the highest （〉2 %）, followed by the refined corn oil （〉1%）, while it was less （〈1%） in the other samples. The results suggested that it was necessary to control the TFAs in fats and oils of pharmaceutical excipients, especially in soybean oil for pharmaceutical use.