Performance Characteristics of Methods of Analysis Used for Regulatory Purposes. I. Drug Dosage Forms. E. Miscellaneous Methods

1985 ◽  
Vol 68 (5) ◽  
pp. 830-838
Author(s):  
William Horwitz ◽  
Richard Albert
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
General Relation ◽  
Drug Dosage ◽  
Dosage Forms ◽  
Allergenic Protein ◽  
Collaborative Studies ◽  
Relative Standard ◽  
Instrumental Methods ◽  
Best Fit

Abstract Precision parameters of miscellaneous methods for the analysis of drug dosage forms approved by AOAC since 1972, and not previously reviewed in this series, were recalculated on a consistent statistical basis by using the computer program FDACHEMIST. Seventeen published collaborative studies were reviewed; the studies encompassed 19 analytes in 80 different materials (dosage forms), 102 collaborative assays, approximately 10 laboratories per study, and principally direct spectrophotometric, polarographic, and spectroscopic methods, for a total of 1451 determinations. The average repeatability relative standard deviation (within-laboratories, RSD„) for the instrumental methods was 1.5%; the reproducibility relative standard deviation (among-laboratories, including within-, RSDX) was 2.6%; the ratio RSD„/RSDX of the averages was 0.57, with an average outlier rate of 2.7% of the reported determinations. The line of best fit of RSDX for the instrumental methods plotted against the negative logarithm of the concentration increases slightly with decreasing concentration, extending from an RSDX of approximately 2.0% at 100% concentration to an RSDX of 3.4% at 0.001% (10 ppm) concentration; this represents an RSDX change of approximately 0.3% (absolute) for each 10-fold decrease in concentration, independent of analyte, matrix, and method. A method for determining precipitated allergenic protein by the micro-Kjeldahl technique appeared to be outside this general relation, showing an RSDX of about 13% at a concentration of 0.015% (150 ppm) nitrogen.

Performance Characteristics of Methods of Analysis Used for Regulatory Purposes. I. Drug Dosage Forms. F. Gravimetric and Titrimetric Methods

1988 ◽  
Vol 71 (3) ◽  
pp. 619-635 ◽  
Author(s):  
Michel Margosis ◽  
William Horwitz ◽  
Richard Albert
Keyword(s):  
Pharmaceutical Preparations ◽  
Drug Dosage ◽  
Drug Analysis ◽  
Dosage Forms ◽  
Fractional Concentration ◽  
Collaborative Studies ◽  
Relative Standard ◽  
The Difference ◽  
Instrumental Methods ◽  
Best Fit

Abstract The original gravimetric and titrimetric methods approved by AOAC for the analysis of pharmaceutical preparations, particularly during the period 1915-1950, show precision, recovery, and outlier parameters approximately the same as those exhibited by the previously reviewed instrumental methods that are currently used. Fifty-nine published collaborative studies utilized gravimetric methods and 85 used titrimetric. The studies of the gravimetric methods encompassed 47 analytes, 95 dosage forms, and 136 assays; the corresponding figures for the titrimetric studies are 72, 112, and 152. An average of approximately 7 laboratories participated per study. The line of best fit of the relative standard deviation between-laboratories (RSDR) plotted against the negative logarithm of the fractional concentration, C, extends from 1.2 and 1.0% for the gravimetric and titrimetric methods, respectively, at 100% concentration to 2.2 and 2.8% at 1.0% concentration. Below this concentration the precision of the titrimetric methods degenerates faster than that of the gravimetric methods. Above about 0.1% concentration the gravimetric and titrimetric methods are somewhat more precise than the instrumental methods in current use for drug analysis. The difference, however, is not statistically significant and the general equation, RSDR = 2 exp(l - 0.5 log C), is also applicable to gravimetric and titrimetric methods above a concentration level of about C = 0.001 (0.1%)

Performance Characteristics of Methods of Analysis Used for Regulatory Purposes.I. Drug Dosage Forms. D. High Pressure Liquid Chromatographic Methods

1985 ◽  
Vol 68 (2) ◽  
pp. 191-198 ◽  
Author(s):  
William Horwitz ◽  
Richard H Albert
Keyword(s):  
High Pressure ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Drug Dosage ◽  
Dosage Forms ◽  
High Pressure Liquid Chromatographic ◽  
Chromatographic Methods ◽  
Collaborative Studies ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract Precision parameters of high pressure liquid chromatographic methods approved by AOAC for the analysis of drug dosage forms were recalculated on a consistent statistical basis, using the computer program "FDACHEMIST." Eleven collaborative studies of 12 compounds in 66 dosage forms analyzed by an average of 9 laboratories per study, with a total of 1150 determinations, were reviewed. For the approved methods and methods awaiting approval (9 studies, 11 compounds, 54 dosage forms, and 959 determinations), the average repeatability relative standard deviation (within-laboratory; RSDo) was 1.0%; reproducibility relative standard deviation (among-laboratories, including within-; RSDX) was 2.5%; the ratio RSD„/RSDX was an unusually low 0.40, with an average outlier rate of 0.6% of the reported values. The line of best fit for RSDX plotted against — log concentration increases with decreasing concentration, extending approximately from RSDX =2% at 100% concentration to RSDX = 3.6% at 0.01% concentration,a change in RSDX of about 0.4% for each 10-fold decrease in concentration,independent of analyte and matrix.

Performance Characteristics of Methods of Analysis Used for Regulatory Purposes. I. Drug Dosage Forms. C. Automated Methods

1985 ◽  
Vol 68 (1) ◽  
pp. 112-121
Author(s):  
William Horwitz ◽  
Richard Albert
Keyword(s):  
Computer Program ◽  
Drug Dosage ◽  
Dosage Forms ◽  
Performance Characteristics ◽  
Methods Of Analysis ◽  
Collaborative Studies ◽  
Relative Standard ◽  
Standard Deviations ◽  
Best Fit ◽  
Automated Methods

Abstract For analysis of drug dosage forms, precision measures of AOAC approved automated methods, usually containing a spectrophotometric or fluorometric measurement step, were recalculated on a consistent statistical basis, using a computer program "FDACHEMIST." Ten collaborative studies of 14 compounds in 38 materials, consisting of various dosage forms, usually in 10 replications by an average of 7 laboratories, with a total of 2461 determinations, were reviewed. The average relative standard deviations within-laboratory (RSD0) and among-laboratories (RSDX) were 1.1 and 1.9%, respectively, and the ratio of RSD„/RSDX was 0.57, with an average outlier rate of 0.57% of the reported values. The line of best fit for RSDX plotted against — log concentration increases slightly with decreasing concentration, extending from an RSDX of about 1.6% at 100% concentration to an RSDX of 2.2% at 0.1% concentration, a change in RSDX of about 0.2% for a 10-fold decrease in concentration, independent of analyte and matrix.

scholarly journals Development and validation of spectrophotometric method for phenylephrine hydrochloride estimation in nasal drops formulations

2008 ◽  
Vol 27 (2) ◽  
pp. 149 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Vladimir Banković
Keyword(s):  
Standard Deviation ◽  
Sodium Hydroxide ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Development And Validation

Simple, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. Phenylephrine hydrochloride was estimated at 291 nm in 1 mol⋅dm-3 sodium hydroxide (pH 13.5). Beer’s law was obeyed in the concentration range of 10–100 μg⋅cm−3 (r2 = 0.9990) in the sodium hydroxide medium. The apparent molar absorptivity was found to be 1.63×103 dm3⋅mol−1⋅cm−1. The method was tested and validated for various parameters according to the ICH (International Conference on Harmonization) guidelines. The detection and quantitation limits were found to be 0.892 and 2.969 μg⋅cm−3, respectively. The proposed method was successfully applied for the determination of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 1 %), while being simple, cheap and less time consuming, and hence can be suitably applied for the estimation of phenylephrine hydrochloride in different dosage forms.

Determination of Nitrate in Vegetables by Continuous Flow: Interlaboratory Study

1994 ◽  
Vol 77 (6) ◽  
pp. 1522-1529 ◽  
Author(s):  
Paul R Beljaars ◽  
Remmelt Van Duk ◽  
Geertrutoa M Van Der Horst
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Continuous Flow ◽  
Collaborative Study ◽  
Leafy Vegetables ◽  
Collaborative Studies ◽  
Relative Standard ◽  
Metallic Cadmium ◽  
Inspection Service

Abstract A collaborative study for the determination of nitrate in leafy vegetables, such as endive, lettuce, spinach, and beetroot, by continuous flow (CF) was conducted by the Project Group on Collaborative Studies of the Inspectorate for Health Protection, Food Inspection Service, in The Netherlands. After extraction with water and filtration, samples were cleaned up by dialysis in the CF system. Extracted nitrates were reduced to nitrite in the system by metallic cadmium, and then the nitrite was reacted with sulfanilamide and N-naphthylethylenediamine to form a reddish-purple azo dye. This dye was measured colorimetrically at 530 nm. Fourteen vegetable samples (including 7 blind duplicates) containing nitrate at ca 900 to 5200 mg/kg were analyzed singly by the proposed procedure by 13 laboratories. The data were analyzed by the International Union for Pure and Applied Chemistry (IUPAC)–International Organization for Standardization (ISO)–AOAC protocol for statistics. One collaborator was identified as an outlier for all results. For all samples analyzed, the repeatability relative standard deviation values varied from 1.7 to 5.5%, whereas the reproducibility relative standard deviation values ranged from 3.3 to 5.9%.

Innovative NSAID dosage forms: lornoxicam suppositories and their standardization

2021 ◽  
pp. 71-76
Author(s):  
Viktoriya Viktorovna Skupchenko ◽  
Ekaterina Nikolaevna Mekhonoshina
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Relative Standard Deviation ◽  
Absorption Spectra ◽  
Dosage Forms ◽  
Uv Spectrophotometry ◽  
Relative Standard ◽  
Standard Solutions

The article presents the studies on the development of a method for the quantitative determination of lornoxime in suppositories using UV spectrophotometry. The optical densities of the test solutions were recorded at a wavelength of 375 nm. The absorption spectra of standard solutions of lornoxicam, as well as of tested solutions of suppositories were obtained. The relative standard deviation was 2.31%.

Performance Characteristics of Methods of Analysis Used for Regulatory Purposes. I. Drug Dosage Forms. B. Gas Chromatographic Methods

1984 ◽  
Vol 67 (3) ◽  
pp. 648-652
Author(s):  
William Horwitz ◽  
Richard Albert
Keyword(s):  
Coefficient Of Variation ◽  
Internal Standard ◽  
Drug Dosage ◽  
Dosage Forms ◽  
Chromatographic Methods ◽  
Collaborative Studies ◽  
Simple Extraction ◽  
Standard Solution ◽  
Best Fit

Abstract Gas chromatographic methods for the analysis of drug dosage forms consist of a simple extraction, dilution with an internal standard solution, and injection, or, even simpler, dilution with the internal standard solution and injection. These methods were used in 7 collaborative studies of the determination of 12 pharmaceuticals, published in the Journal of the AOAC during 1973–1983. A total of 43 individual materials consisting of various dosage forms were each analyzed, usually in duplicate, by an average of 8 laboratories, with a total of 582 reported determinations. The average within-laboratory coefficient of variation (CVo) was 1.25% and the average among-laboratories coefficient of variation (CVx) was 2.41%, for a CVo/CVx ratio of 0.52, at an average outlier rate of 1.4% of the reported values. The line of best fit for CVx plotted against concentration increases with decreasing concentration, extending from a CVx of approximately 1.8% at 100% concentration to a CVx of approximately 3.2% at 1% concentration. The change in CVx for a 10-fold decrease in concentration is approximately 0.7% CVx, independent of analyte and matrix.

Determination of Bismuth in Pharmaceutical Dosage Forms by Conventional DC Polarography

1972 ◽  
Vol 55 (1) ◽  
pp. 155-160
Author(s):  
William M Plank
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Dosage Forms ◽  
Official Method ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard ◽  
Dc Polarography

Abstract A method has been investigated for the determination of bismuth in pharmaceutical dosage forms by conventional dc polarography. The method is applicable to tablets, emulsions, suspensions, injectables, and bulk powders. A collaborative study has shown the method to be superior in accuracy and precision to the present official colorimetric method, 36.300- 36.304. The results from 16 determinations performed by 8 collaborators were: 100.0±1.5% recovery on a synthetic powder mix, a relative standard deviation of 1.9% on a commercial tablet sample, and a relative standard deviation of 2.1% on a magma sample. By comparison, the collaborative data reported for the present official method gave relative standard deviations of 3.4 and 3.2% on 2 samples of powder mixtures. It is recommended that the polarographic method be adopted as official first action.

Precision Parameters of Standard Methods of Analysis for Dairy Products

1989 ◽  
Vol 72 (5) ◽  
pp. 784-806 ◽  
Author(s):  
James T Peeler ◽  
William Horwitz ◽  
Richard Albert
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Freezing Point ◽  
Milk Products ◽  
Standard Methods ◽  
Methods Of Analysis ◽  
Collaborative Studies ◽  
Relative Standard ◽  
Repeatability And Reproducibility

Abstract The available collaborative studies for standard methods of analysis for various constituents of milk and milk products were examined in an attempt to assign specific repeatability and reproducibility precision parameters to these methods. The different collaborative assays for the primary constituents (moisture/solids, fat, protein), the nutritionally important elements (calcium, sodium, potassium, phosphorus), and miscellaneous analytes/physical constants (ash, lactose, salt, freezing point) produced different estimates of the precision parameters for the same method. A suitable summary of the precision estimates from collaborative studies is given by the reproducibility relative standard deviation, RSDR, which is relatively constant within a product and permits comparisons across products. An estimate of the variation of RSDR for an analyte from a number of collaborative studies is presented in terms of the median and 90% interval (the range of the centermost 90% of values). These estimates are only informative when a substantial number of independent studies are available for pooling the independent estimates to form a distribution of RSDR values. The RSDR for the determination of the primary constituents of milk and milk products is characterized by a median RSDR of 1% and a 90% interval of 0.3-3%, with RSDR estimates occasionally occurring below 0.3% and above 4%. These overall estimates appear to be independent of analyte, matrix, and method and apply to concentrations of primary constituents that range from about 2 to 80%. The repeatability relative standard deviation, RSDR, is unstable, although it tends to converge to about 0.5-0.7 X RSDR. Too few collaborative assays are available to characterize RSDR for the determination of certain other constituents (acidity, ash, lactose, salt, and the nutritionally important elements) unless RSDR values for different analytes, methods, and matrixes are pooled on the basis of similar analyte concentrations. When pooled, the RSDR values are generally better than predicted from the Horwitz equation, RSDR (%) = 2 exp (1—0.5 logioC), where C is the concentration expressed as a decimal fraction; all but one of 661 RSDR values are within the upper empirical limit of twice this curve.

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate

Sign in / Sign up

Export Citation Format

Share Document