摘要
建立测定大米中石蜡的气相色谱-串联质谱(GC-MS/MS)法。样品经石油醚提取,浓缩后用正己烷溶解,加浓硫酸净化,通过对C_(24)、C_(26)、C_(28)、C_(30)、C_(33)5种烷烃的测定,进行石蜡的定性分析,用上述5种烷烃的峰面积之和进行定量分析。该方法的检出限为0.25mg/kg,定量限为0.75mg/kg,加标回收率及精密度实验的平均回收率为93.38%~110.22%,相对标准偏差(RSD)为5.42%~12.11%,相关系数为0.9980。结果表明,该方法精密度良好,检测结果可靠,可作为大米中石蜡的测定方法。
A method for the determination of paraffin in rice by GC-MS/MS was established. The samples were extracted with petroleum ether, condensed, dissolved with n-hexane, and purified by concentrated sulfuric acid. The paraffin was qualitatively analyzed by the determination of 5 alkanes including C_(24), C_(26), C_(28), C_(30) and C_(33), and quantitatively analyzed by the sum of the peak area of 5 alkanes. The detection limit of the method was 0.25 mg/kg,and the limit of quantitation was 0.75 mg/kg, the standard recovery rate and the average recovery rate of the precision experiments were 93.38%-110.22%,the relative standard deviation(RSD) was 5.42%-12.11%, and the correlation coefficient was 0.9980. The results showed that the precision of the method was good, the results were reliable, and the method could be used for the determination of paraffin in rice.
引文
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