ABSTRACT
A Fast Chemical Identification System (FCIS) consisting of two colour reactions based on functional groups in molecules of macrolide antibiotics and two TLC methods was developed for screening of fake macrolide drugs. The active ingredients could be extracted from their oral preparations by absolute alcohol. Sulfuric acid reaction as a common reaction of macrolides was first used to distinguish the macrolides from other types of drugs and then 16-membered macrolides and 14-membered ones were distinguished by potassium permanganate reactions depending on the time of loss of colour in the test solution; after which a TLC method carried out on a GF(254) plate (5 cm x 10 cm) was chosen to further identification of the macrolides. The mobile phase A consisting of ethyl acetate, hexane and ammonia (100:15:15, v/v) was used for the identification of 14-membered macrolides, and the mobile phase B consisting of trichloromethane, methanol and ammonia (100:5:1, v/v) was used for the identification of 16-membered ones. A suspected counterfeit macrolide preparation can be identified within 40 min. The system can be used under different conditions and has the virtues of robustness, simplicity and speed.
Subject(s)
Anti-Bacterial Agents/analysis , Chemistry, Pharmaceutical/methods , Chromatography, Thin Layer/methods , Drug and Narcotic Control/methods , Fraud/prevention & control , Macrolides/analysis , Pharmaceutical Preparations/analysis , Ammonia/analysis , Chemistry Techniques, Analytical/methods , Chloroform/analysis , Chromatography, High Pressure Liquid , Consumer Product Safety , Hexanes/analysis , Hydrolysis , Models, Chemical , Potassium Permanganate/analysis , Sulfuric Acids/analysisABSTRACT
AIM: To study the crystalline characteristics of ceftezole sodium. METHODS: Ceftezole sodium crystals were obtained from different solvents. X-ray diffraction, DSC, TGA, etc were used to analyze the crytals. RESULTS: Ceftezole sodium crystal was easily obtained in isopropanol-water mixture. It consists of ceftizole sodium monohydrate, which consists of type I and type II two different crystal forms. Powder X-ray diffraction patterns showed differences between type I and the type II crystal forms. Peaks at 8 degrees and 18 degrees in diffractograms of the type I, but at 9 degrees and 18.6 degrees in the type II could be observed. Water molecules in different crystal forms had different combining condition. They lost during 35-117 degrees C in the type I form, but lost during 110-160 degrees C in the type II form. CONCLUSION: Structure of ceftizole sodium monohydrate crystal obtained in different circumstance could be some vary, which influence upon the thermal stability of the compound. The type I crystal form is more stable than the type II.
