头孢匹林钠原料药及注射剂中头孢匹林、去乙酰头孢匹林和头孢匹林内酯的稳定性指示液相色谱测定法

Stability-indicating liquid chromatographic determination of cephapirin, desacetyl cephapirin and cephapirin lactone in sodium cephapirin bulk and injectable formulations.

作者信息

MacNeil L, Rice J J, Muhammad N, Lauback R G

出版信息

J Chromatogr. 1986 Jun 27;361:285-90. doi: 10.1016/s0021-9673(01)86917-x.

Abstract

A specific, stability-indicating, high-performance liquid chromatographic assay was developed for the determination of cephapirin, desacetyl cephapirin and cephapirin lactone in sodium cephapirin (cefadyl) bulk and injectables. The procedure uses a muBondapak C18 column and a mobile phase of dimethylformamide-acetic acid-potassium hydroxide in water. UV detection at 254 nm is used for quantitation with acetanilide used as the internal standard. The assay is precise, accurate and linear over the range of 100-300 micrograms/ml for cephapirin and over the range of 2-6 micrograms/ml for desacetyl cephapirin and cephapirin lactone. The assay is also stability-indicating for the described thermal, acid, base, aqueous and accelerated light degradations.

摘要

已开发出一种特定的、指示稳定性的高效液相色谱法，用于测定头孢匹林钠（先锋霉素Ⅰ）原料药和注射剂中的头孢匹林、去乙酰头孢匹林和头孢匹林内酯。该方法使用μBondapak C18柱和水相中的二甲基甲酰胺 - 乙酸 - 氢氧化钾流动相。采用254 nm处的紫外检测进行定量，以乙酰苯胺作为内标。该测定法在头孢匹林浓度为100 - 300微克/毫升、去乙酰头孢匹林和头孢匹林内酯浓度为2 - 6微克/毫升的范围内精确、准确且呈线性。该测定法对所述的热、酸、碱、水和加速光降解也具有指示稳定性的作用。