顶空气相色谱法测定头孢替坦二钠中的残留溶剂

Determination of Residual Solvents in Cefotetan Disodium by Headspace Gas Chromatography

目的建立测定头抱替坦二纳原料药中9种残留溶剂的方法。方法使用DB-624毛细管柱（30m x0. 32 mm，1. 8μm） 为色谱柱，以水为溶剂，测定头抱替坦二纳原料药中甲醇、丙刷、乙腊、二氯甲炕、丁嗣、乙酸乙醋、四氢吹喃的含量;使用HPFFAP毛细管柱（25 m x0. 32 mm，0. 5μm）为色谱柱，以20%的二甲亚矶为溶剂，测定头抱替坦二纳原料药中苯甲诞、异辛酸 的含量。结果甲醇、丙嗣、乙腊、二氯甲：皖、丁闹、乙酸乙醋、四氢吹喃、苯甲隧、异辛酸分离度良好;在所考察的浓度范围内线性关系良好，r分别在0.9988-0.9997之间;3个水平的回收率分别在95.71 % - 103. 55%之间，RSD分别在0.39＇1毛-2.289毛 之间。结论两种方法均准确、灵敏，可用于头抱替坦二纳原料药中残留溶剂的测定。

OBJECTIVE To establish a method for determining nine residual solvents in cefotetan dis odium by heads pace gas chromatography. METHODS The residual solvents including methanol, acetone, acetonitrile, dichloromethane, butanone, ethyl acetate, tetrahydrofuran in cefotetan disodium were quantitatively determined on a DB-624 column （30 m X 0. 32 mm, 1. 8 ILm）. Water was solvent media. The residual solvents of anisole and isocaprylic acid in cefotetan disodium were quantitatively determined on a HPFF AP column （25 m x 0. 32 rnm , 0. 5 μm）. The 20% dimethylsulfoxide （ DMSO） was used as the solvent. RESULTS Nine residual solvents were completely separated. Good linearity of the solvents were obtained within the determination ranges. There between O. 998 8 and o. 999 7. The average recoveries of three levels were in the range of 95.71 % - 103. 55%. The RSDs were 0.39% - 2.28%. CONCLUSION The established two methods are accurate and sensitive, and can be used for the determination of residual solvents in cefotetan disodium.