摘要
目的建立顶空-毛细柱气相色谱内标法测定食用植物油中六号溶剂残留量的检测方法。方法以氮气为载气,采用气液顶空气相色谱法,试样在70℃,平衡30 min后经HP-5毛细柱分离,FID检测,正庚烷内标法定量,测定试样中六号溶剂残留量含量。结果六号溶剂含量在10 mg/kg～200 mg/kg内线性关系良好,相关系数均≥0.999 80,方法检出限为0.70 mg/kg。配制20.0 mg/kg、50.0 mg/kg、200.0 mg/kg 3个不同浓度加标样品并平行进样6次,其平均回收率为95.1%～103.0%,相对标准偏差为3.1%～4.4%。结论本方法操作简单,自动化程度高,分离效果好,灵敏度高,重现性好,在较宽的线性范围内有良好的准确度和精密度,结果准确可靠,可应用于日常工作中食用植物油中六号溶剂残留量的检测分析。
Objective To establish an auto headspace capillary gas chromatography method with internal standard for the determination of No.6 solvent residual in edible vegetable oil.Methods Based on the auto headspace sampling method,N2 was adopted as the carrier gas.The samples were separated by the HP-5 capillary column after balanced at 70℃ for 30 minutes,and then monitored by the detector of FID and quantified by the n-heptane internal standard.Results It showed the good linearity was obtained within 10 mg/kg-200 mg/kg,with the correlation coefficients all above 0.999 8.The detection limits of the method was 0.70 mg/kg.The recoveries of 20.0 mg/kg,50.0 mg/kg and 200.0 mg/kg ranged from 95.1% to 103.0%,with RSD of 3.1 %-4.4%.Conclusion This method is simple,automatic,accurate and precise.It is suitable for the determination of No.6 solvent residual in edible vegetable oil.
作者
雷凯
王芳
王建国
LEI Kai;WANG Fang;WANG Jian-guo(Physics and Chemistry Laboratory,Tongzhou Center for Disease Control and Prevention,Beijing 101100,China)
出处
《中国卫生检验杂志》
CAS
2019年第7期795-797,共3页
Chinese Journal of Health Laboratory Technology
关键词
顶空气相色谱法
内标法
六号溶剂残留量
食用植物油
Headspace gas chromatography
Internal standard
No.6 solvent residual
Edible vegetable oil
作者简介
雷凯(1980-),男,本科,主管技师,主要从事理化检验工作。
