坚果中微量氰化物的顶空气相色谱法测定  

Determination of trace cyanide in nuts by headspace gas chromatography

作　　者：徐毅[1] 龚文杰[1] 陈海燕[2] XU Yi;GONG Wen-jie;CHEN Hai-yan(Cixi Municipal Center for Disease Control and Prevention,Cixi,Zhejiang 315300,China)

机构地区：[1]慈溪市疾病预防控制中心,浙江慈溪315300 [2]慈溪市妇幼保健院,浙江慈溪315300

出　　处：《中国卫生检验杂志》2020年第12期1432-1434,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立顶空气相色谱法测定坚果中微量氰化物的方法。方法采用0.1%NaOH碱液浸泡坚果8 h后的提取液,用氯胺T将提取液中的氰化物衍生化为氯化氰,直接顶空进样,经INNOWAX气相色谱柱(30 m×0.25 mm,0.25μm)分离,气相色谱法ECD检测器检测,外标法定量。同时对检测方法中的浸提时间、衍生酸度、衍生剂用量、顶空保温温度及时间等气相色谱条件进行优化。结果氰化物在0.001 mg/L^0.100 mg/L内具有良好的线性,相关系数可达到0.999,方法检出限为0.05 mg/kg,定量限为0.15 mg/kg。加标回收率在87.2%~104.2%,相对标准偏差值RSD为3.9%~5.7%。结论本法操作简便快捷,具有良好的重现性、较高的灵敏度,可用于坚果中微量氰化物含量的分析检测。Objective A method based on headspace gas chromatography has been developed for the determination of trace cyanide in nuts.Methods The extract was soaked in nuts with 0.1%NaOH lye for 8 hours.The cyanide in the extract was derivatized with chloramine T to cyanogen chloride.The headspace sample was injected directly through INNOWAX gas chromatography column(30 m×0.25 mm,0.25μm)separation,gas chromatography ECD detector,external standard method for quantification.At the same time,the gas chromatographic conditions such as leaching time,derivatized acidity,amount of derivatizing agent,headspace holding temperature and time in the detection method were optimized.Results Cyanide has good linearity in the range of 0.001 mg/L to 0.100 mg/L,the correlation coefficient can reach 0.999,the detection limit of the method is 0.05 mg/kg,and the limit of quantification is 0.15 mg/kg.The recoveries of spiked standards ranged from 87.2%to 104.2%,and the relative standard deviation value(RSD)was within 3.9%-5.7%.Conclusion The method is simple,reproducible,sensitive,and it is suitable to the determination of cyanide in nuts.

关 键 词：顶空气相色谱法 坚果 氰化物 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]