摘要
该研究通过优化前处理和色谱条件,建立一种气相色谱-质谱联用(GC-MS)检测牛乳中1,2-丙二醇的方法。结果表明,样品采用乙腈提取,分散固相萃取法净化,DB-WAX色谱柱(30 m×0.25 mm×0.25μm)分离,分流比10∶1,采用选择离子监测(SIM)模式,进行GC-MS测定,外标法定量。在此条件下,1,2-丙二醇在1.0~50μg/m L质量浓度范围内线性关系良好,相关系数(R^(2))>0.999,牛乳中1,2-丙二醇的检出限(LOD)为0.005 g/kg,定量限(LOQ)为0.010 g/kg,加标回收率为93.67%~100.67%,精密度试验结果的相对标准偏差(RSD)为1.23%~3.91%。该方法前处理简便、抗基质干扰能力强、结果准确、对仪器的污染损害小,具有一定的推广价值,可用于牛乳中1,2-丙二醇检测。
A method for the detection of 1,2-propanediol in milk by gas chromatography-mass spectrometry(GC-MS)was established by optimizing pretreatment and chromatographic conditions.The results showed that the samples were extracted with acetonitrile,purified by dispersion solid-phase extraction,separated by DB-WAX chromatographic column(30 m×0.25 mm×0.25μm)with a split ratio of 10:1,determined by GC-MS using the se-lective ion monitoring(SIM)mode,and quantified by the external standard method.Under these conditions,1,2-propanediol had a good linear rela-tionship within the mass concentration range of 1.0-50μg/ml,with a correlation coefficient(R)>0.999.The detection limit(LOD)of 1,2-propanediol in milk was 0.005 g/kg,and the limit of quantification(LOQ)was 0.010 g/kg.The recovery rate of standard addition was 93.67%-100.67%,and the relative standard deviation(RSD)of the precision test results was 1.23%-3.91%.This method featured simple pretreatment,strong resistance to matrix interference,accurate results,and minimal contamination and damage to the instrument.It had certain promotion value and could be used for the de-tection of 1,2-propanediol in milk.
作者
高玉杰
张立佳
李培珍
吴晓莉
莫楠
白艳梅
汪洋
刘丽君
GAO Yujie;ZHANG Lijia;LI Peizhen;WU Xiaoli;MO Nan;BAI Yanmei;WANG Yang;LIU Lijun(Inner Mongolia Yili Industrial Group Co.,Ltd.,Hohhot 010110,China;Key Laboratory ofCattle and Sheep Milk and Meat Products Risk Control and Key Technology,State Administration for Market Regulation,Hohhot 010110,China)
出处
《中国酿造》
北大核心
2025年第9期261-266,共6页
China Brewing
基金
国家市场监督管理总局重点实验室项目(991100000380)。
