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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 gas chromatography-mass spectrometry was developed for the determination of trans fatty acids in medicinal oils and fats to improve the quality standards of medicinal oils and excipients. After the sample was esterified, the gas chromatography was performed on a SP-2560 elastic quartz capillary column with an inlet temperature of 250 ° C and a programmed temperature ramp. The mass spectra were qualitatively detected by Scanning Electron Impact (EI) ion source in Scan mode (m / z 40 ~ m / z 390) and single ion monitoring (SIM) mode to eliminate background interference for quantification with more sensitivity high. Apply this method to test quality control samples of Fapas (Food Analysis Performance Assessment Scheme) to verify the feasibility and accuracy of the method. Results | z | <2. The method was applied to the determination of trans-fatty acids in seven kinds of oil samples, including pharmaceutical excipients and edible soybean oil, corn oil, peanut oil and olive oil. The results showed that 52 fatty acids were completely separated. The total content of trans fatty acids in medicinal soybean oil is higher (> 2%); followed by refined corn oil, the total content is more than 1%; the other five kinds of oil samples contain less than 1% of total trans fatty acids. The results show that it is necessary to control the trans fat in pharmaceutical excipients, especially soybean oil.