气相色谱-质谱联用测定南瓜籽油中角鲨烯的含量

Determination of squalene in pumpkin seed oil by gas chromatography-mass spectrometry

基于GB/T 22110—2008方法,建立一种简单、快速测定南瓜籽油中角鲨烯含量的气相色谱-质谱联用（GC-MS）方法,考察了甲酯化试剂浓度对角鲨烯提取效果及不同极性色谱柱对角鲨烯分离程度的影响,确定南瓜籽油中角鲨烯含量测定的最佳条件。结果表明,0.2 g南瓜籽油经1 m L0.5 mol/L的氢氧化钾-甲醇溶液进行甲酯化反应,正己烷提取后经极性色谱柱HP-FFAP分离,用GC-MS选择离子监测模式对角鲨烯可以进行定量测定。该方法在10~500 mg/L范围内线性关系良好,相关系数r=0.999 9;检出限为0.12 mg/kg,加标回收率为79.33%~91.33%,平均相对标准偏差为3.99%。采用该方法测定的14种市售南瓜籽油中角鲨烯平均含量为1.44 g/kg。

A simple and rapid method for the determination of squalene in pumpkin seed oil by gas chromatography - mass spectrometry（ GC - MS） was developed based on the national standard GB/T 22110-- 2008. The optimal determination conditions were obtained through studying the effects of dosage of methyl esterification reagent on the extraction result of squalene and different polarity columns on the separation degree of squalene. The results showed that after pumpkin seed oil （0.2 g） was methyl esterified by 1 mL 0.5 mol/L potassium hydroxide -methanol solution and then extracted by n -hexane, the product was separated by HP - FFAP column, now the squalene could be determined quantitatively by GC - MS in selective ion monitoring mode. The linear range, correlation coefficient, the limit of detection, recovery rate of standard addition and average relative standard deviation of the method were 10 - 500 rag/L, 0. 999 9,0.12 mg/kg, 79.33% -91.33% and 3.99%, respectively. The average content of squalene of 14 kinds of commercial pumpkin seed oils determined by the method was 1.44 g/kg.