顶空固相微萃取-气相色谱-质谱法测定面包中曲酸的含量

Determination of Crotonic Acid in Bread by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry

本文建立了顶空固相微萃取-气相色谱-质谱法测定面包中的曲酸含量,并优化顶空条件以及进行方法学验证测定。结果表明,当平衡温度为90℃、平衡时间为30 min时,曲酸的标准曲线方程为Y=0.1903X+0.0046,r^(2)为0.9996,保留时间为12.175 min。曲酸的平均加标回收率为92.51%~96.49%,相对标准偏差为9.0%~10.2%。该方法具有线性关系良好、回收率和精密度高等优点,可用于面包中曲酸的定量检测。

In this paper,a headspace solid-phase microextraction-gas chromatography-mass spectrometry method was developed for the determination of trichothecenes in bread.The determination was carried out by optimizing the headspace conditions as well as performing methodological validation.The results showed that when the equilibrium temperature was 90℃and the equilibrium time was 30 min,the standard curve equation of crotonic acid was Y=0.1903X+0.0046,r^(2) was 0.9996,and the retention time was 12.175 min.The average spiked recoveries of crotonic acid were in the range of 92.51%~96.49%with the relative standard deviations of 9.0%~10.2%.The method has the advantages of good linearity,high recovery and precision,and can be used for the quantitative determination of crotonic acid in bread.