摘要
建立顶空进样-气相色谱测定维生素D滴剂中甲醇、乙醇、异丙醇、正丁醇、二氯甲烷、丙酮、乙酸乙酯、丁酮、苯、甲苯、2-乙烯苯、正己烷12种溶剂残留量的分析方法。采用CD-624毛细管色谱柱分离,平衡温度为80℃,平衡时间为30 min,分流比为3∶1,用氢火焰离子化检测器检测,以色谱峰面积内标法定量。12种残留溶剂在0~10mg/kg范围内,线性相关系数均大于0.999,方法检出限为0.3~0.5 mg/kg,定量限为0.6~1.0 mg/kg。样品加标回收率为83.57%~97.80%,测定结果的相对标准偏差均小于10%(n=6)。该方法简单、快速,可满足维生素D滴剂中溶剂残留量的检测。
A method was established to determine the residual amounts of 12 solvents in vitamin D drops by headspace injection gas chromatography,including methanol,ethanol,isopropanol,n-butanol,dichloromethane,acetone,ethyl acetate,butanone,benzene,toluene,2-ethylbenzene,and n-hexane.CD-624 capillary chromatography column was used as separation column,with an equilibrium temperature of 80℃,equilibrium time of 30 min,and a split ratio of 3∶1.Hydrogen flame ionization detector was used to determine and quantification was performed using an internal standard method for chromatographic peak area.The linear correlation coefficients of 12 residual solvents were all more than 0.999 in the range of 0-10 mg/kg.The detection limits of the method were 0.3-0.5 mg/kg,and the quantitative limits were 0.6-1.0 mg/kg.The recoveries of sample spiking were 83.57%-97.80%,and the relative standard deviations of the measurement results were all less than 10%(n=6).The method is simple and fast,and it can meet the detection of solvent residue in vitamin D drops.
作者
顾璇
李灿
崔艳华
武蕊
唐文杰
陈同强
GU Xuan;LI Can;CUI Yanhua;WU Rui;TANG Wenjie;CHEN Tongqiang(Department of Pharmacy,3201 Hospital of Xi'an Jiaotong University Health Science Center,Hanzhong 723000,China;Hunan Province Produce Commodity Quality Testing&Research Institute,Changsha 410007,China)
出处
《化学分析计量》
CAS
2024年第5期6-11,共6页
Chemical Analysis And Meterage
基金
湖南省自然科学基金项目(2022JJ90024,2022JJ90026)。
作者简介
通信作者:李灿,工程师,硕士,主要从事食品安全技术研究。
