Determination of Squalene in Vegetable Oil by Gas Chromatography-Mass Spectrometry and Methods Comparison
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摘要: 建立气相色谱-质谱联用法（Gas chromatography mass spectrometry，GC-MS/MS）分离和测定植物油料中角鲨烯的方法。用氢氧化钾-乙醇溶液超声皂化后，正己烷溶液萃取，氮吹浓缩，正己烷溶解，提取物经HP-5MS柱分离后进入质谱仪检测，外标法定量。该方法在角鲨烯浓度0.1~100.0 mg/L的范围内具有良好的线性关系（r=0.9998），方法的精密度良好RSD为1.00%~3.35%，加标回收率为83.60%~110.44%，平均加标回收率为98.89%，方法的检出限（RSN=3）为0.10 mg/L。通过气相色谱质谱联用与气相色谱对四类实际油料样品的分析表明，气相色谱质谱联用方法具高效快速、操作简单、污染小以及检测灵敏度高等优点，可以满足植物油料中角鲨烯的快速、高通量检测。Abstract: A method for separation and determination of squalene in plant oil by gas chromatography-mass spectrometry(GC-MS/MS)was established. After ultrasonic saponification with potassium hydroxide-ethanol solution,the n-hexane solution was extracted and concentrated with nitrogen blowing,and the n-hexane was dissolved. The extract was separated by an HP-5MS column and then detected by a mass spectrometer,and quantified by an external standard method. The method had a good linear relationship(r=0.9998)in the range of squalene concentration 0.1~100.0 mg/L,the RSD of the method was 1.00%~3.35%,and the recovery rate of spiked was 83.60%~110.44%,the average recovery rate of spiked was 98.89%,and the detection limit(RSN=3)of the method was 0.10 mg/L. The analysis of four types of actual oil samples by gas chromatography-mass spectrometry and gas chromatography showed that the gas chromatography-mass spectrometry method has the advantages of high efficiency and rapidity,simple operation,low pollution,and high detection sensitivity,which can meet the rapidity of squalene in vegetable oil,high-throughput detection.
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