摘要
采用顶空气相色谱法,建立帕瑞昔布钠中6种残留溶剂的测定方法.试样以N,N-二甲基甲酰胺(DMF)为溶剂,应用程序升温来测定.结果显示,乙醇、二氯甲烷、乙酸乙酯、正己烷、4-二甲氨基吡啶、三乙胺的定量限分别为5. 42μg、5. 62μg、5. 49μg、0. 3μg、3. 19 ng、0. 69μg;在0. 00965~6. 372 mg/m L范围内,各溶剂的峰面积与浓度呈良好的线性关系,平均回收率分别为100. 57%~104. 07%,RSD为0. 68%~2. 47%;方法完全适合用于本品的残留溶剂的测定.
A method for determining the six residual organic solvents in parecoxib sodium is developed on headspace GC. Temperature programming is used for determination while N, N-Dimethylformamide（DMF） are taken as the solvent. The results show that the quantitative limits of ethyl alcohol, methylene dichloride, ethyl acetate, normal hexane, 4-dimethylaminopyridine, and triethylamine are 5.42 μg, 5.62μg, 5.49μg, 0.3 μg, 3.19 ng,0.69 μg respectively. The concentrations of the solvents are linear with the peak areas in the range of 0.00965 mg/mL- 6. 372 mg/mL. It is concluded that the average recovery rate is 100.57 % - 104.07 % （RSD： 0.68 % - 2.47 % ）. The method is suitable for the determination of the residual solvent in parecoxib sodium.
作者
聂忠莉
毛玉萍
王晓玲
萧茂玲
张勇
黄金玉
郭瑞
NIE Zhongli;MAO Yuping;WANG Xiaoling;XIAO Maoling;ZHANG Yong;HUANG Jinyu;GUO Rui(School of Pharmacy and Bioengineering,Chengdu University,Chengdu 610106,China;Chengdu Climb Pharmaceutical Technology Co.,Ltd.,Chengdu 610041,China)
出处
《成都大学学报（自然科学版）》
2018年第3期260-263,共4页
Journal of Chengdu University（Natural Science Edition）
关键词
帕瑞昔布钠
残留溶剂
气相色谱法
方法学验证
parecoxib sodium
residual solvent
gas chromatography
method validation
