Drug preparations, analysis

The acceptance criterion for recovery data is 98-102% or 95-105% for drug preparations. In biological samples, the recovery should be 10%, and the range of the investigated concentrations is 20% of the target concentrations. For trace level analysis, the acceptance criteria are 70-120% (for below 1 ppm), 80-120% (for above 100 ppb), and 60-100% (for below 100 ppb) [2]. For impurities, the acceptance criteria are 20% (for impurity levels <0.5%) and 10% (for impurity levels >0.5%) [30], The AOAC (cited in Ref. [11]) described the recovery acceptance criteria at different concentrations, as detailed in Table 2. A statistically valid test, such as a /-test, the Doerffel-test, or the Wilcoxon-test, can be used to prove whether there is no significant difference between the result of accuracy study with the true value [29],... 

DNLM 1. Combinatorial Chemistry Techniques--methods. 2. Drug Design. 3. Pharmaceutical Preparations—analysis. 4. Technology, Pharmaceutical—methods. QV 744 H6366 2009]... 

In many developing countries of the world, there is still a major reliance on crude drug preparation of plants used in traditional medicines for their primary health care. Pharmacognosists employed in the different institutions are aware of the changing trends of herbal medications and a number of useful texts on the analysis, uses, and potential toxicities of herbal remedies have appeared recently, which serves as useful guides in pharmacy practice. The history of medicine includes many ludicrous therapies. Nevertheless, ancient wisdom has been the basis of modem medicine and will remain as one important source of future medicine and therapeutics. The future of natural products drug discovery will be more holistic, personahzed and involve the wise use of ancient and modem therapeutic skills in a complementary manner so that maximum benefits can be accmed to the patients and the community. 

Sample preparation procedures commonly used in the field of drug residues analysis are briefly described below. Since some of these overlap and cannot be strictly separated, the intent of the authors is to attempt to outline the complexity of die sample preparation issue rather than to give a comprehensive listing of the relevant literature. 

Immunoaffinity cleanup was first applied in drug residue analysis for the determination of chloramphenicol in swine muscle tissue by LC (113). The lAC column was prepared using monoclonal antibodies originally developed for an enzyme-linked immunosorbent assay (ELISA) method (171) specific for chloramphenicol. Meat samples were extracted with water, and a concentrated phosphate buffer was added to the filtered extracts before immunoaffinity cleanup. A phosphate buffer was used in the washing process, whereas chloramphenicol was eluted from the column with a glycine/sodium chloride solution of pH 2.8. For subsequent LC analysis, this eluate was extracted with ethyl acetate, evaporated, and reconstimted in the mobile phase. The same analytical scheme was later successfully applied for the determination of chloramphenicol in eggs and milk as well (170, 172). 

Alekseichik, et al (139) have published qualitative analysis of vitamin Bg and other drug preparations. The spectra are determined in ethanol, hydrochloric acid, and sodium hydroxide, using vitamin Bg concentrations from 0.01-0.001 mg/ml. 

An impressive variety of LC/MS-based solutions, incorporating quantitative and qualitative process approaches, are now routinely applied to accelerate drug development. The results are significant and led to the successful development of innovative therapies and numerous novel drugs. The use of LC/MS with other technologies for sample preparation, analysis, and data management is now an inextricably linked element of drug development. 

G. V. Failonde and S. N. Joshi, Analysis of a drug preparation containing nosapine, ephedrine hydrochloride and chlorpheniramine maleate by thin layer chromatography, Indian Drugs, 23 515 (1986). 

However signs do change with the "handedness" of the natural isomer so a higher level of distinction is achieved using CD or polarimetric detection. An enormous advantage is derived from the fact that achiral excipients, such as lidocaine, procaine, and benzocaine, often deliberately added to illicit drug preparations to complicate the chromatographic identifications of amphetamine and methamphetamine, present no interference problem whatsoever to CD detection. ORD detection was developed for the analysis of mixtures of pseudoephedrine and ephedrine [47], which because of the connection between anomalous ORD and CD, should be applicable to CD detection in the UV. 

The refractive index detector is inherently insensitive (as much as 100 times less sensitive than UV detectors) and this severely limits its use in drug analysis. However, it can be used when the compounds of interest do not have a suitable ultraviolet chromophore and are present in high concentration, e.g. sugars in drug preparations (B. B. Wheals and P. C. White, J. Chromat., 1979,176, 421-426). 

The sample for examination may be the parent drugin a pharmaceutical preparation or illicit drug preparation, or may be the drug together with a metabolite in a complex biological sample. In the latter case, some degree of clean-up/separation is required prior to mass spectrometric analysis. 

In drug preparations, sensitivity is not a particular problem as there is always sufficient of the active constituent present. Suitable extraction procedures should be carried out and each fraction should then be subjected to chromatographic analysis. The mass spectra, together with the appropriate retention parameters, may then be used for identification purposes. In many cases mass spectrometric analysis is undertaken as confirmation of an identification based on the physical characteristics such as size, colour, markings, etc., of the tablet or capsule. Mass spectrometry may be used not only to identify the major components but also the trace impurities. This information may be used for quality control purposes, and may enable the route of manufacture of certain drugs to be determined. 

Finally, impurity analysis can also be utilized to demonstrate illegal use of patented reaction routes. The impurity profile of a drug substance is influenced by the synthetic route and the source and quality of the starting materials. Identification of impurities in drug prepared by two different manufacturers may provide valuable insight into the manufacturing route and determine if patent infringement has occurred, because certain impurities may be indicators of a specific synthetic route. 

Many publications dealing with TLC-HPTLC steroid analysis have appeared every year. The publications can be summarized into categories as follows analytical control of steroid formulations (drug preparations), determination of steroids in biological media and natural resources, and analytical control of the production of steroids (including raw material, syntheses, and biotransformation). A cumulative database of thousands of TLC methods (including steroids) is provided in compact-disk (CD) format by Camag [6]. 

The initial concentration of active principle in an aqueous preparation was 5.0 x 10 g cm . After 20 months the concentration was shown by analysis to be 4.2 x 10 g cm . The drug is known to be ineffective after it has decomposed to 70% of its original concentration. Assuming that decomposition follows first-order kinetics, calculate the expiry date of the drug preparation. 

Newer methods of chemical analysis led to the isolation of the major alkaloids from crude drug preparations. By 1833, aconitine, atropine, codeine, hyoscyamine, morphine, nicotine, and strychnine had been isolated from plants. Color tests for alkaloids were developed between 1861 and 1882 by 1890 quantitative analysis methods became available. Physiological tests for alkaloids, particularly strychnine, first used in 1856, were employed well into the twentieth century. Tests for alcohol, devised by Lieben (iodoform crystal test, 1870) and others, were later perfected for the quantitative analysis of alcohol in body fluids and tissues. Qualitative tests for carbon monoxide in the blood were developed about this time and in 1880, Fodor developed a palladium chloride reduction method to quantitate carbon monoxide in blood. 

DNLM 1. Pharmaceutical Preparations-analysis-Handbooks. 2. Pharmaceutical Preparations-analysis-Laboratory Manuals. 3. Drug Contamination-prevention Sc control-Handbooks. 4. Drug Contamination-prevention Sc control-Laboratory Manuals. 5. Pharmaceutical Preparations-standards-Handbooks. 6. Pharmaceutical Preparations-standards—Laboratory Manuals. 7. Technology, Pharmaceutical—methods—Handbooks. 8. Technology, Pharmaceutical— methods-Laboratory Manuals. QV 25 H2364 2003]... 

For each herbal drug preparation, a comprehensive specification must be submitted. This must be established on the basis of recent scientific data and must give particulars of the characteristics, identification tests, and purity tests. This has to be done, for example, by the appropriate chromatographic methods. If deemed necessary by the results of the analysis of the starting material, tests on microbiological quality, residues of pesticides, fumigation agents, solvents, and toxic metals have to be carried out. Radioactivity should be tested if there are reasons for concerns. Quantitative determination (assay) of markers or of substances with known therapeutic activity is required. The content must be indicated with the lowest possible tolerance. The test methods must be described in detail. 

Sample Preparation Perspectives in Drug Product Analysis... 

The recovery of a sample preparation must be assessed, because the recovery determines the accuracy of the analysis. For drug substance and drug product analysis, recovery of 100% is generally required to maintain required levels of accuracy and precision. For biological samples, less than quantitative recovery is generally acceptable if the recovery is reproducible. 

TLC) is widely used for the rapid analysis of drugs and drug preparations. There are... 

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