果蔬中柠檬烯GC法和GC-MS法测定条件优化研究

Optimization of Pretreatment and Chromatographic Methods in limonene Determination

针对目前果蔬中柠檬烯的快速准确检测所面临的难题,本文采用DB-1色谱柱分离及FID检测方法,对10种水果和5种蔬菜中的柠檬烯进行定性和定量测定,并对提取柠檬烯的前处理条件及色谱和质谱条件进行优化,同时对2种方法的线性、回收率、精密度和灵敏度进行实验验证,实验结果表明,2种方法均有良好的线性关系（r＞0.99）,GC法的定量限为0.5 mg/kg,加标回收率为90.6％～95.9％,相对标准偏差为2.13％.GC-MS法的定量限为0.2 mg/kg,加标回收率为89.1％～98.5％,相对标准偏差为3.24％.2种方法操作简便,回收率较高,精密度良好,且这2种方法的测定结果无显著性差异,均可用于蔬菜和水果等食品中柠檬烯的测定.

To deal with the challenge of how to rapidly and accurately detect limonene in fruits and vegetables,we use a column of DB-1 to separate and to detect with GC-FID,10 kinds of fruits and 5 kinds of vegetables had been detected,and sample pretreatment had been optimized.Linear correlation,recovery,precision and sensitivity had been validated simultaneously.The experimental results showed a good linear relationship between the peak area and the concentration （r＞0.99）,the recoveries for limonene were 90.6％～95.9％ for GC and 89.1％～98.5％ for GC-MS,and the relative standard deviation（RSD） was 2.13％ for GC and 3.24％ for GC-MS,the LOQ was 0.5mg/kg for GC and 0.2mg/kg for GC-MS.The results show that the two methods have no notable diversity and both are simple,rapid,accurate and suitable for analysis of limonene in fruits and vegetables.