杏仁及其制品中氰化物的顶空气相色谱测定法

Determination of cyanide in almond and almond products by headspace gas chromatography

建立测定杏仁及其制品中氰化物的顶空气相色谱(HS-GC)法,为食品风险监测提供参考。杏仁及其制品中的氰化物经水解和提取,在酸性条件下用氯胺T将其衍生为氯化氰,经顶空进样,气相色谱电子捕获检测器检测,外标法定量。结果显示:氰化物的质量浓度在0.001~0.050μg·mL^(-1)内与其对应的峰面积成线性关系(r=0.9998),方法的检出限(LOD)为0.03 mg·kg^(^(-1)),定量限(LOQ)为0.1 mg·kg^(-1);在低、中、高3种添加水平下,平均回收率为99.0%~108.5%,相对标准偏差(RSD)为2.7%~8.7%。该方法简单、高效、灵敏度高、准确性好,适用于杏仁及其制品中氰化物的测定。

This thesis established a headspace gas chromatography(HS-GC)method for determination of cyanide in almond and almond products to provide reference for food risk monitoring.The samples were hydrolysed and extracted,and then derived into cyanogen chloride by chloramine T in acid condition.The cyanogen chloride was analyzed by HS-GC,quantitatived by external standard method.The results showed that linear relationship between values of peak area and mass concentration of cyanogen chloride was kept in the range of 0.001 to 0.050μg·mL(r=0.9998),with the limit of detection(LOD)was 0.03 mg·kg and the limit of quantitation(LOQ)was 0.1 mg·kg.At the spiked concentration of low,middle and high levels,mean recoveries of cyanide in almond and almond products ranged from 99.0 to 108.5%,with the relative standard deviation(RSD)ranging from 2.7%to 8.7%.The proposed method is simple,sensitive,and accurate,which could meet the monitoring requirements of cyanide in almond and almond products.