方法学研究-中国药品标准.PDFVIP

D rug Standards of China 20 10, V ol11 N o3 20 10 11 3 199 1 2 1 1 1 1 刘冬 , 战寒秋 , 王茜, 金笃嘉 , 冯文华 , 兰 培 ( 1, 100050; 2, 100015 ) : 建立了测定西维来司钠中甲醇正己烷 酸 酯四氢呋喃甲苯吡啶N, N二甲基甲酰胺残留有机溶剂含量 的顶空气相色谱法: 采用顶空气相色谱法, F D 检测器, 以二甲基亚砜为溶媒, 醇为内标, 顶空预热温度为 85 , 预热 时间为 30 m in, 进样口温度为 180 , 检测器温度为 250 , 以氮气为载气, 在 C P S L 5CB 的 60 m ! 032 mmid, 膜厚为 1 m 的交联毛细管柱上, 应用程序升温, 实现了各组份的基线分离: 在甲醇正己烷 酸 酯四氢呋喃甲苯吡啶N , N 二甲基甲酰胺各自对应的浓度范围内, 线性关系良好; 各组分最低检测限分别为 10 , 01, 08, 10, 08, 10, 100 mg L- 1 加样回收率 ( n = 5) 分别为 978% ( RSD = 082% )964% ( R SD = 11% )981% ( R SD = 093% ) 967% ( RSD = 18% ) 10 15% ( RSD = 13% )963% ( RSD = 19% )952% ( R SD = 24% ), 精密度较好: 经方法学验证, 该方法灵敏准确 可靠, 适用于西维来司钠中甲醇正己烷 酸 酯四氢呋喃甲苯吡啶N, N二甲基甲酰胺等残留溶剂的测定 : 顶空气相色谱法; 西维来司钠; 残留溶剂测定 : 9212 : A : 1009- 3656( 20 10) - 3- 199- 4 Determination ofResidualSolvents in SivelestatSodium byHeadSpaceGasChromatography 1 2 1 1 1 1 L iu Dong , Zhan H anqiu , W ang X i, J in DuJ ia , Feng W enH ua , Lan Pe i ( 1Institu te of M a teria M ed ica Ch ineseA cad emy of M ed ical S cien ce s, Beji ing 100050; 2B eij ing D itan H osp ita ,l B eij ing 100015 Abstract Objective: Th is paper reports a G C m e thod for determ ination ofm ethano,l hexane, ethy l ace tate, tetrahydrofuran, m e thy l benzene, pyridine and dmi ethyl form am ide in Sivelestat Sodium Method: T he ana ly tica l co lum n w as CP S L 5CB ( 60 mm ! 032 mm, 10 m ) T he injector tem pe ra ture w as 180 , and the detecto r temperature was 250 T he co lum n tem perature w as pro g ramm ed ra ised T he carrier gas w as nitrogen, and the so lvent was d mi ethy l su lfox ideResults: T he standard curves w ere linear fo r m ethanol, hexane, ethy l acetate, tetrahydrofuran , m ethy lbenzene, py