摘要
建立了气相色谱-氢火焰离子化检测法(GC-FID)对牛奶中1,2-丙二醇的含量进行测定的方法。采用FID检测器,用DB-WAX(30 m×0.32 mm×0.25μm)毛细管色谱柱分离,外标法定量。结果表明,在2~100μg/mL范围内1,2-丙二醇线性关系良好,相关系数R2达到0.9998;以3倍信噪比(S/N=3)设定1,2-丙二醇的检出限为2.8 mg/kg;样品加标回收率为90.41%~98.99%,相对标准偏差RSD(%)为0.81%~1.82%;储存实验中,离心管中储存(室温或冷藏)的样品溶液在12 h内或进样瓶中储存的样品滤液在24 h内,1,2-丙二醇含量稳定,满足日间检测要求;超声30 min的样品处理方式,与GB 5009.251-2016相比,提取率提高了15.33%。本方法操作简单、检出限低、重现性好、回收率高,同时提高了检测效率,适合牛奶中1,2-丙二醇的批量样品检测,也为其他食品中1,2-丙二醇含量检测提供参考。
A method for the determination of 1,2-propanediol in milk was established by gas chromatographyhydrogen flame ionization detector(GC-FID).The targeted analyte was detected by FID detector,separated by DB-WAX(30 m×0.32 mm×0.25μm)capillary column and quantified with external standard method.The results showed that the linear relationship of 1,2-propanediol was good within the concentration range of 2〜100μg/mL,the correlation coefficient(R2)was 0.9998;The detection limit of 1,2-propanediol was 2.8 mg/kg at signal-tonoise ratio 3;The recovery of 1,2-propanediol was 90.41%〜98.99%,and the relative standard deviation RSD(%)was 0.81%〜1.82%;In the storage experiment,the content of 1,2-propanediol was stable when being stored in the centrifuge tube(room temperature or refrigeration)within 12 h or in the injection vial within 24 h,met the requirements of daytime detection.Compared with the method of national standard GB 5009.251-2016,the extraction rate of samples treated by ultrasound for 30 min increased 15.33%.The GC-FID method had the characteristics of simple operation,low detection limit,good repeatability and high recovery rate,the detection efficiency was improved at the same time.It is suitable for batch sample detection of 1,2-propanediol in milk,and also provides reference for the determination of 1,2-propanediol content in other foods.
作者
张云林
李正新
ZHANG Yunlin;LI Zhengxin(Huaibei Food and Drug Inspection Center,Huaibei 235000)
出处
《中国食品添加剂》
CAS
北大核心
2023年第9期279-285,共7页
China Food Additives
