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. 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.

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.

scholarly journals Liquid Chromatographic Determination of Ampicillin Residues in Porcine Muscle Tissue by a Multipenicillin Analytical Method: European Collaborative Study

2002 ◽  
Vol 85 (4) ◽  
pp. 889-900 ◽  
Author(s):  
Eric Verdon ◽  
Pierric Couëdor ◽  
Pierre Maris ◽  
Michel Laurentie ◽  
P Batjoens ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Muscle Tissue ◽  
Phosphate Buffer ◽  
Collaborative Study ◽  
Porcine Muscle ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A collaborative study involving 14 laboratories was conducted to determine residues of ampicillin in porcine muscle tissue by using a liquid chromatographic method developed for multipenicillin analysis that can quantitate 8 penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, amoxicillin, nafcillin, oxacillin, cloxacillin, and dicloxacillin) at trace levels in muscle tissue. This method involves extraction of the penicillins with phosphate buffer, pH 9, followed cleanup and concentration on a C18 solid-phase extraction column and reaction with benzoic anhydride at 50°C and with 1,2,4-triazole and mercury(II) chloride solution, pH 9.0, at 65°C. The derivatized compounds are eluted isocratically on a C8 column with a mobile phase of acetonitrile and phosphate buffer (pH 6; 0.1M) containing sodium thiosulfate and the ion-pair reagent tetrabutylammonium hydrogen sulfate. The penicillins are detected by UV absorption at 325 nm. The limit of detection and the limit of determination (quantitation) of the method were calculated to be approximately 3–5 and 25 μg/kg, respectively, in accordance with the criteria of European Union (EU) Decision No. 93/256/EEC. In this first interlaboratory study, collaborators were instructed to monitor 4 different penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, and amoxicillin) by analyzing 8 blind samples of muscle tissue in triplicate. These samples were prepared from 2 materials containing different concentrations of incurred ampicillin (63.5 μg/kg for material No. 1 and 358.1 μg/kg for material No. 2) and 1 blank material. The repeatability relative standard deviation and the reproducibility relative standard deviation were 10.2 and 17.4%, respectively, for material No. 1 and 7.0 and 16.0%, respectively, for material No. 2. These results demonstrate that the method is suitable for the determination of ampicillin residues in muscle tissue at the EU maximum residue limit (50 μg/kg) and above. However, the identification of positives by this procedure may need additional confirmation by techniques with greater specificity, such as liquid chromatography combined with mass spectrometry, or tandem mass spectrometry. Investigations regarding the basis of interlaboratory testing studies will further demonstrate the suitability of multiresidue methodology for detecting and quantitating other compounds in the family of penicillin antibiotics.

scholarly journals Liquid Chromatographic Determination of Deoxynivalenol in Baby Food and Animal Feed: Interlaboratory Study

2006 ◽  
Vol 89 (4) ◽  
pp. 1012-1020 ◽  
Author(s):  
Joerg Stroka ◽  
Michelle Derbyshire ◽  
Carsten Mischke ◽  
Massimo Ambrosio ◽  
Katy Kroeger ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Animal Feed ◽  
Chromatographic Determination ◽  
Baby Food ◽  
Interlaboratory Study ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract An interlaboratory study was conducted for the determination of deoxynivalenol in baby food and animal feed by high-performance liquid chromatography with UV detection. The study included 14 participants representing a cross section of industry, official food control, and research facilities. Mean recoveries reported ranged from 89% (at 120 g/kg) to 85% (at 240 g/kg) for baby food and from 100% (at 200 g/kg) to 93% (at 400 g/kg) for animal feed. On the basis of the results for spiked samples (blind duplicates at 2 levels), as well as those for naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) in analyses of baby food ranged from 6.4 to 14.0% and in analyses of animal feed, from 6.1 to 16.5%. The relative standard deviation for reproducibility (RSDR) in analyses of baby food ranged from 9.4 to 19.5% and in analyses of animal feed, from 10.5 to 25.2%. The HorRat values ranged from 0.4 to 1.0 and from 0.7 to 1.3, for baby food and animal feed, respectively. The method showed acceptable performance for within-laboratory and between-laboratory precision for each matrix, as required by European legislation.

High Pressure Liquid Chromatographic Determination of Melengestrol Acetate in Dry Feed Supplements

1981 ◽  
Vol 64 (3) ◽  
pp. 661-664
Author(s):  
Jose E Roybal
Keyword(s):  
High Pressure ◽  
Standard Deviation ◽  
Methylene Chloride ◽  
Animal Feed ◽  
Confirmatory Test ◽  
High Pressure Liquid Chromatographic ◽  
Melengestrol Acetate ◽  
Feed Supplements ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method is described for the quantitative determination of melengestrol acetate (MGA) in dry animal feed supplements containing 0.000027-0.000220% MGA (0.125-1.00 mg/lb). Ground feed is Soxhletextracted with hexane, and the extract is partitioned from hexane into aqueous methanol and then into methylene chloride, followed by mixed column chromatography. MGA is then quantitated by HPLC. Average recovery of standard MGA through the method at 1.00 ppm (0.454 mg/lb).was 94.8% with a 3.58% standard deviation. Average spike recovery of MGA in fortified feed at 0.100 ppm (0.0454 mg/lb) to 2.00 ppm (0.907 mg/lb) level was 97.8% with a standard deviation of 5.39%. In addition, the method includes a 2-dimensional thin layer chromatographic confirmatory test for MGA.

High Pressure Liquid Chromatographic Method for Probenecid in Flavored Oral Suspensions Containing Ampicillin: Collaborative Studies

1978 ◽  
Vol 61 (3) ◽  
pp. 687-694
Author(s):  
Paul J Vollmer ◽  
Thomas G Alexander ◽  
Carol Haneke
Keyword(s):  
High Pressure ◽  
Linear Response ◽  
Chromatographic Method ◽  
Random Order ◽  
High Pressure Liquid Chromatographic ◽  
Collaborative Studies ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic method for determining probenecid in oral suspensions of amoxicillin was applied to the determination of probenecid in oral suspensions of ampicillin. Three preparations containing various known amounts of probenecid in synthetic mixtures of ampicillin oral suspensions were analyzed by 5 chemists in an intralaborastory study, with satisfactory results. Blind duplicates of 3 prepared oral suspensions were sent to 12 collaborators, who were instructed to analyze the samples in a fixed random order. The standards showed a satisfactory linear response. Average recoveries of probenecid in the interlaboratory study for the 6 mixtures ranged from 95.2 to 99.1%, and the coefficients of variation ranged from 1.63 to 4.9%.

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%.

Comparison of GLG and High-pressure Liquid Chromatographic methods for Analysis of Urinary Pseudoephedrine

1979 ◽  
Vol 68 (11) ◽  
pp. 1472 ◽  
Author(s):  
David M. Baaske ◽  
Chii-Ming Lai ◽  
Lawrence Klein ◽  
Zee M. Look ◽  
Avraham Yacobi
Keyword(s):  
High Pressure ◽  
High Pressure Liquid Chromatographic ◽  
Chromatographic Methods ◽  
Liquid Chromatographic

scholarly journals High-pressure-liquid-chromatographic analysis of tetracarboxylic porphyrins in hepatic porphyrias

1982 ◽  
Vol 207 (3) ◽  
pp. 599-603 ◽  
Author(s):  
Anthony H. Jackson ◽  
K. R. Nagaraja Rao ◽  
Sydney G. Smith
Keyword(s):  
High Pressure ◽  
Quantitative Analysis ◽  
Chromatographic Analysis ◽  
High Pressure Liquid Chromatographic ◽  
Chromatographic Methods ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

New high-pressure-liquid-chromatographic methods have been developed for the quantitative analysis of mixtures of coproporphyrins I and III, and of isocoproporphyrin, dehydroisocoproporphyrin and de-ethylisocoproporphyrin.

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