气相色谱法测定维生素K1中残留溶剂含量.doc

气相色谱法测定维生素K1中残留溶剂含量[摘要] 目的：测定维生素K1中甲醇、正己烷、乙酸乙酯和甲苯的含量。方法：采用毛细管气相色谱法，OV-101色谱柱，程序升温，载气为氮气，检测器为FID，外标法计算含量。结果：在选定的色谱条件下，测得各有机溶剂的含量与峰面积线性关系良好（r＞0.99）；甲醇、正己烷、乙酸乙酯和甲苯的平均加样回收率分别为100.60%、98.65%、101.42%、101.62%。三批样品中4种有机溶剂残留量均符合规定。结论：经方法学验证，该方法灵敏、准确，适用于本品有机溶剂残留的测定。 [关键词] 维生素K1；有机溶剂残留；气相色谱法 [中图分类号]R927 [文献标识码]A [文章编号]1673-7210（2008）07（b）-035-02 Determination of residual organic solvents in Vitamin K1 by gas chromatography MAO Ying1, BI Zhong-zhou1, DENG Zhi-jian2 (1.Henan Sunny Pharmaceutical Co. LTD., Kaifeng 475000, China;2.The First Affiliated Hospital of Xinxiang Medical College, Weihui 453100, China) [Abstract] Objective: To determine the contents of the residual methanol, n-hexane, ethyl acetate and toluene in Vitamin K1. Methods:The capillary gas chromatography method was established with FID detector. The capillary column was OV-101 with programmed temperature rising. The carrier gas was nitrogen, the residues were calculated by an external standard method. Results:The linearity of all the four solvents was fairly good. The average recoveries of methanol, n-hexane, ethyl acetate and toluene were 100.60%, 98.65%, 101.42%, 101.62% respectively.The contents of the four residual organic solvents in three bathes of samples all reached the standard requirements. Conclusion:The method is proved to be accurate, sensitive and reliable.It is suitable for the test analysis of the four kinds of solvents. [Key words] Vitamin K1; Residual organic solvents; Gas chromatography 维生素K1是脂溶性维生素，应用广泛。但维生素K现行的药品标准中亦未修订其残留溶剂项。由于维生素K1在生产过程中使用到国际协调组织(ICH)规定的二类溶剂甲醇（限度为0.3%），正己烷（限度为0.029%），甲苯（限度为0.089%）和三类溶剂乙酸乙酯（建议限度为0.5%），故应在质量标准中加以监控。笔者报道的气相色谱法专属性强，能在同一试验中同时测定四种溶剂的含量，程序升温，方法简便准确。 1 仪器与试药 GC1102气相色谱仪配手动进样装置（上海分析仪器厂）；OV-101 毛细管柱(30 m ×0.53 mm×10 μm，大连化物所)。 甲醇（分析纯，上海振兴化工一厂，批；正己烷[分析纯，中国医药(集团)上海化学试剂公司，批号071022]；甲苯[分析纯，中国医药(集团)上海化学试剂公司，批号071202]；乙酸乙酯[分析纯，中国医药(集团)上海化学试剂公司，批号070103]；二甲亚砜[分析纯，中国医药(集团)上海化学试剂公司，批号070523]；维生素K1原料（河南大明制药有限公司，批号070701）。 2 方法与结果