United States Pharmacopoeia analysis

Test Methods. In addition to that provided by proper sampling and rephcation of analysis, a test method also has a significant impact on the accuracy and precision of the results. Preferred methods are those which are accepted in the chemical industry such as those from the American Society of Testing Materials (ASTM), Association of Official Analytical Chemists (AO AC), or from compendia such as the United States Pharmacopoeia (USP) or the Pood Chemical Codex (FCC) (36). The use of such methods eliminates the need for method vahdation. 

United States Pharmacopoeia 28 [1] describes a microbiological method under antibiotics-microbial assays for the analysis of OTC and nystatin capsules, OTC and nystatin for oral suspension, OTC HC1 and hydrocortisone ointment, and OTC HC1 and polymyxin B sulfate ointment. The methods are relative rather than absolute, which are based on the determination of the level of oxytetracycline by a microbiological response to a series of standard oxytetracycline concentrations by a... 

The United States Pharmacopoeia 23 [11] and Indonesian Pharmacopoeia IV [9] describe the assay of benzoic acid and salicylic acid in ointments. Two chromatographic columns (20 x 2.5 cm) are used to effect the separation. One transfers a mixture of 1 g siliceous earth and 0.5 mL diluted phosphoric acid (3 in 10) to the first column (A), then packs above this a mixture of 4 g siliceous earth and ferric chloride-urea reagent. A mixture of 4 g siliceous earth and 2mL of sodium bicarbonate solution (1 in 12) is packed into the second column (B). For analysis, column A is mounted directly above column B. The sample solution is inserted onto column A, allowed to pass into the column, and then washed with 2-40 mL of chloroform. Benzoic acid can be eluted from column B by using a 3 in 100 solution of glacial acetic acid in chloroform. The benzoic acid content then can be determined by a spectrophotometric method such as that described earlier (section 4.5). 

The use of GC was first included in the United States Pharmacopoeia (USP) in the sixteenth edition in 1960, and became an official method of the British Pharmacopoeia (BP) in 1968. GC has found widespread use in pharmaceutical analysis by virtue of its applications to purity and control analysis of raw materials, content and quality assessment of dosage forms (including product stability), and in the quantitative measurement of drugs in biological fluids. The latter application is important for therapeutic drug monitoring, pharmacokinetic studies, and bioavailability assessments. In fact, in a survey on GC use, ° a major application of this technique was in the field of pharmaceuticals. 

Paul, L. Personal Communication, Associate Director, General Policies, Nomenclature and Labeling Division United States Pharmacopoeia Rockville, MD, 2000. Hinshaw, J.V. Headspace sampling. LC-GC 1990, 8, 362. Jack, D.B. Drug Analysis by Gas Chromatography Academic Press New York, 1984. 

United States Pharmacopoeia Rev. 25 and National Formulary Rev. 20. 2002 General Test (891) Thermal Analysis, p. 2081. 

Another calculation method to evaluate peak asymmetry can be found in the different pharmacopoeias, for example, United States Pharmacopoeia (USP) or Pharmacopoeia Europea (PhEUR). These pharmacopoeias calculate peak tailing from an analysis at 5% of the peak height (Equation 2.20) ... 

The United States Pharmacopoeia has many well-established protocols for the analysis of drug compounds. See Table 5.5 for details [590]. 

The official methods (pharmacopoeial methods) in this respect are different from the methods used in the industrial analysis. For example, in the United States Pharmacopoeia, HPLC is the primary method and TLC the second choice. Application of the methods used for purity testing in the British Pharmacopoeia is different TLC is the primary method, and HPLC is the second choice. But, both Pharmacopoeias are in agreement that conventional TLC is used without instrumentation. In the industrial pharmaceutical analysis, HPLC and instrumental TLC are more or less used equally and in many cases in conjunction. 

USP (United States Pharmacopoeia and National Formulary). Column descriptions of the analysis of specific targeted analytes are provided in Table 2.15. 

Solubility of the dosage form is a key factor when it comes to analysis. Solubility is expressed as the concentration of a substance in a saturated solution at a defined temperature. The United States Pharmacopoeia (USP) defines solubility as shown in Table 1. The nature of the API may be such that it may be nonionizable and so poorly soluble in water but its corresponding salts may be ionizable and as a consequence become water soluble." Depending on the nature of the dosage form, the first step in the sample preparation technique to employ is to determine what type of solvent system will be best to achieve maximum solubility of the API in the presence of excipients. Maximum solubility of the API ensures that its recovery from the sample preparation steps will be an accurate measure of drug content in the pharmaceutical dosage form. 

Nevertheless, there is an individual monograph for each active ingredient published in the United States Pharmacopoeia (USP) under its United States Adopted Name (US AN) this includes specifications and verification methods. However, the USP does not outline the methods necessary to detect OTC drug ingredients in the finished product. It is the responsibility of each supplier to define such methods. The FDA simply indicates that these products must be open to analysis and states the acceptance criteria to be taken into... 

Methods of Analysis and Excipient Monographs, in 1989 the Ph Eur. the Japanese Pharmacopoeia (JP), and the United States Pharmacopeia (USP) formed a Pharmacopoeial Discussion Group (PDG) (for details of the PDG process see Table 16.3). However, progress is slow. At the time of... 

Infrared spectra are now widely used in the examination of pharmaceuticals. The sixteenth revision of The Pharmacopoeia of the United States (U.S.P.) and the eleventh edition of the National Formulary (N.F.) have presented identification tests which used infrared spectroscopy, whereas no infrared tests were used in U.S.P. XV or N.F. X. Infrared spectra have attained acceptance in legal considerations and are now given in patent applications as characteristics of antibiotics of unknown structure. In the pharmaceutical industry there are many applications for quantitative infrared analyses in research and development work, pharmacy research, and in various phases of pharmaceutical production. For example, infrared data are used to characterize reaction conditions and yields, to assay the purity of intermediate products, to examine such problems as the stability of a drug in the material in which it is suspended, and to maintain quality control in the chemical production of bulk drugs. A recent review (Papendick et al, 1969) has given many references to fractionation and isolation methods for pharmaceutical analysis, such as the various types of chromatography, electrophoresis, countercurrent distribution, and extraction. The authors presented many references to infrared analyses for a wide variety of compounds (Table 16.1). 

This chapter reviews only those aspects of steroid TLC analysis that have been published during the last ten to fifteen years (1980-1994). Not every aspect of steroid analysis has been considered. This review focuses mainly on steroid analysis in industry, and distinction is made to the methods prescribed in various pharmacopoeias, i.e., the United States Pharmacopeia, 22nd edition (USP XXn), the British niarmacopoeia edition 1988 (BP88), and the European pharmacopoeia (Ph. Eur). This review to sununarizes the most important sinailarities and differences between the various pharmacopoeias TLC methods. 

The various pharmacopoeias and codices have a major influence on the control of the purity of drugs and any textbook on drug analysis must take cognisance of the methods in current official publications. The necessarily frequent publication of new pharmacopoeias is occasioned by the new drugs available rather than by advances in analytical chemistry this edition is correlated with the British Pharmacopoeia 1958 and the United States Pharmacopeia XVI, but since it includes the latest trends in analytical techniques its contents should cover official methods for quantitative... 

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