Kalmár E, Kormányos B, Szakonyi G, Dombi G
Institute of Pharmaceutical Analysis, Faculty of Pharmacy, University of Szeged, H-6720 Szeged, Somogyi u. 4., Hungary.
Generic R&D Division, TEVA Pharmaceuticals Ltd, Debrecen, H-4042 Debrecen, Pallagi út 13., Hungary.
Indian J Pharm Sci. 2014 Jan;76(1):31-7.
Suppositories are important tools for individual therapy, especially in paediatrics, and an instrumental assay method has become necessary for the quality control of dosage units. The aim of this work was to develop a rapid, effective high-performance liquid chromatography method to assay aminophenazone in extemporaneous suppositories prepared with two different suppository bases, adeps solidus and massa macrogoli. With a novel sample preparation method developed by the authors, 4-dimethylaminoantipyrine was determined in these suppository bases with 95-105% recovery. The measurements were carried out on a Shimadzu Prominence ultra high-performance liquid chromatography system equipped with a 20 μl sample loop. The separation was achieved on a Hypersil ODS column, with methanol, sodium acetate buffer (pH 5.5±0.05, 0.05 M, 60:40, v/v) as the mobile phase at a flow rate of 1.5 ml/min. The chromatograms were acquired at 253 nm. The chromatographic method was fully validated in accordance with current guidelines. The presented data demonstrate the successful development of a rapid, efficient and robust sample preparation and high-performance liquid chromatography method for the routine quality control of the dosage units of suppositories containing 4-dimethylaminoantipyrine.
栓剂是个体化治疗的重要工具，尤其是在儿科领域，因此对于栓剂剂型的质量控制而言，一种仪器分析方法已成为必要。本研究的目的是开发一种快速、有效的高效液相色谱法，用于测定用两种不同栓剂基质（硬脂和聚乙二醇基质）制备的临时用栓剂中的氨基苯乙酮。通过作者开发的一种新型样品制备方法，在这些栓剂基质中测定了4-二甲基氨基安替比林，回收率为95-105%。测量在配备20 μl进样环的岛津Prominence超高效液相色谱系统上进行。在Hypersil ODS柱上进行分离，以甲醇、醋酸钠缓冲液（pH 5.5±0.05，0.05 M，60:40，v/v）作为流动相，流速为1.5 ml/min。在253 nm处采集色谱图。该色谱方法已按照现行指南进行了全面验证。所提供的数据表明，已成功开发出一种快速、高效且稳健的样品制备和高效液相色谱法，用于含4-二甲基氨基安替比林栓剂剂型的常规质量控制。
