scholarly journals VALIDATION OF THE SPECTROPHOTOMETRIC PROCEDURE FOR DESLORATADINE ASSAY IN TABLETS APPLYING THE UNCERTAINTY CONCEPT OF THE STATE PHARMACOPOEIA OF UKRAINE

2020 ◽  
pp. 74-87
Author(s):  
Dmytro Leontiev ◽  
Vasyl Petrus ◽  
Natalia Volovyk ◽  
Oleksandr Gryzodub
Keyword(s):  
Confidence Interval ◽  
Analytical Procedure ◽  
Pharmaceutical Preparation ◽  
Pilot Scale ◽  
The State ◽  
Intermediate Precision ◽  
Single Experiment ◽  
Target Uncertainty ◽  
Spectrophotometric Procedure ◽  
Accuracy And Precision

Aim. This work aimed to validate an assay procedure for desloratadine tablets by direct spectrophotometric method. Materials and methods. A pilot-scale batch of the pharmaceutical preparation Alerdez, film-coated tablets containing 5 mg of desloratadine, manufactured by PJSC SIC “Borshchahivskiy CPP”, Ukraine, was used as an object of the study. A UV-Vis spectrophotometer Lambda 25 (Perkin Elmer), analytical balance Mettler Toledo XP 205DR, and class A volumetric apparatus were used in the study. Validation of the procedure was performed following the metrological approach of the State Pharmacopoeia of Ukraine (SPhU), whose requirements for the target uncertainty and bias, which rest on the risk assessment of making incorrect decisions on compliance (a confidence level of 95 %), were translated into criteria for all validation characteristics recommended by ICH. All calculations were made in normalised coordinates. The linearity, accuracy and precision (repeatability) were studied in a single experiment using nine different concentrations that uniformly covered the range of ±30 % from the nominal concentration of desloratadine. For validation of the procedure, an SPhU reference standard of desloratadine was used. Results. The experiment design and validation characteristics being tested were in full compliance with ICH Q2(R1) recommendations. All performance characteristics conformed to the criteria recommended by the SPhU. Requirements for the target uncertainty (1.6 %) and bias for any systematic source of variation (≤0.51 %, negligible in relation to 1.6 %) were established. The analytical procedure was specific – the absorbance from the placebo solution was insignificant (A %=0.36). The procedure met the requirements for linearity, accuracy, and precision at the repeatability level. The residual standard deviation s0 was 0.34 (≤ 0.84); correlation index Rc was 0.9998 (≥0.9991); intercept а was 0.045 (less than its confidence interval ∆a=1.14). The confidence interval for recovery ∆Z, which was used as a precision estimate, was 0.55 % (less than the target uncertainty). The mean recovery, which was used as an accuracy estimate, statistically insignificantly deviated from 100% (|Zmean ‑ 100| = 0.022 %).  The confidence interval for the intermediate precision ∆intra was 0.33 % (less than the target uncertainty). The developed analytical procedure was found to be robust. Conclusions. A spectrophotometric procedure suitable for the assay of desloratadine in film-coated tablets Alerdez with content limits of ±5 % was validated by the SPhU approach.

Analytical and technical aspects of testing for drug abuse: confirmatory procedures.

1988 ◽  
Vol 34 (3) ◽  
pp. 471-473 ◽  
Author(s):  
M A Peat
Keyword(s):  
Drug Testing ◽  
Analytical Procedure ◽  
Gas Chromatography Mass Spectrometry ◽  
Technical Aspects ◽  
Governmental Agencies ◽  
Accuracy And Precision ◽  
Urine Drug Testing ◽  
Urine Drug ◽  
Chemical Technique ◽  
Layer Chromatography

Abstract Many laboratories are now performing urine drug testing for employers, governmental agencies, and other institutions. It is now recognized that presumptive positive screening results have to be confirmed by an analytical procedure based on a different chemical technique with greater than or equal sensitivity to the screening test. Thin-layer chromatography has been widely used for this; however, it is relatively insensitive for certain drugs, and it cannot satisfy the accuracy and precision requirements needed to determine threshold concentrations reliably. Gas chromatography-mass spectrometry is able to satisfy these threshold requirements and has become the method of choice for confirming initial immunoassay results.

scholarly journals Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

scholarly journals Reconsidering the Estimation of Salmon Mortality Caused by the State and Federal Water Export Facilities in the Sacramento–San Joaquin Delta, San Francisco Estuary

2020 ◽  
Vol 18 (3) ◽  
Author(s):  
Andrew Jahn ◽  
William Kier
Keyword(s):  
San Francisco ◽  
Chinook Salmon ◽  
Near Field ◽  
San Francisco Estuary ◽  
The State ◽  
Juvenile Salmon ◽  
Small Fish ◽  
Accuracy And Precision ◽  
Behavioral Barriers ◽  
Existing Data

Combined water exports from Old River in the south end of California’s San Francisco Estuary (estuary) by state and federal pumping facilities entrain small fishes, including out-migrating juvenile salmon. Both export projects have fish salvage facilities that use behavioral barriers (louvers) in combination with screens to guide fish into collection areas from which they are trucked to release points in the western Delta. Sacramento River-origin Chinook Salmon are regularly taken in the projects’ fish salvage operations. Survival has been estimated within the boundaries of both intake structures, but not in Old River. Prevailing methods for estimating fish losses are based on studies of louver efficiency, near-field survival at the state facility, and assumed survival at the federal facility. The efficiency of the fish salvage operations is affected by several factors, including intake velocity, debris build-up on the louvers and trash racks, and by the omnipresence of predators in front of and within the fish guidance structures. Analysis of existing data suggests that under average conditions, juvenile salmon survive entrainment into the forebay of the state facility at a rate of less than 10%. There is no evidence for better survival at the federal facility. We found no data on predation outside of either the state’s forebay or the federal trash boom, structures which are separated by an approximately 2-km reach of Old River where predation on small fish is thought to be intense. We suggest an improvement to the existing loss estimation, and discuss some features of the studies needed to increase its accuracy and precision.

Should More Polls Be Interpreted as Too Close to Call?

2013 ◽  
Vol 46 (02) ◽  
pp. 329-332
Author(s):  
Walter W. Hill
Keyword(s):  
Confidence Interval ◽  
Confidence Level ◽  
Political Campaigns ◽  
The State ◽  
Horse Race ◽  
Percentage Points ◽  
Margin Of Error ◽  
The Difference

AbstractDuring political campaigns the spread between the popularity of the candidates is a common metric capturing the state of the horse-race feature of the campaign. One candidate is said to be ahead of another by an indicated number of percentage points. If the difference is less than the margin of error, the race is considered too close to call. In two-person races, however, the spread corresponds to a much smaller confidence level than is usually reported because the two numbers used to compute the spread are not independent. The size of the confidence interval that is typically reported is incorrect by a factor of two. Therefore, some spreads that are reported as decisive are races too close to call.

scholarly journals DEVELOPMENT AND VALIDATION OF A TLC DENSITOMETRIC METHOD FOR DETERMINATION OF GLIMEPIRIDE IN TABLETS

2014 ◽  
Vol 16 (1) ◽  
pp. 11-15
Author(s):  
Yuni Retnaningtyas ◽  
Lestyo Wulandiri ◽  
Gabriella F Punu
Keyword(s):  
Pharmaceutical Analysis ◽  
Data Recovery ◽  
Antidiabetic Drug ◽  
Intermediate Precision ◽  
Quantification Limit ◽  
Accuracy And Precision ◽  
Quality Control Testing ◽  
The Mean ◽  
Development And Validation

A simple and valid TLC method has been developed for the determination of glimepiride in tablet formulation. After extraction of the analyte with a mixture of methanol and ammonia 0,2M (1:1, v/v), the extracts were spotted on precoated TLC silica gel F254 plates, which were developed with a mixture of toluene:methanol:ethyl acetate (75:20:5, v/v/v). Quantitative evaluation was performed by measuring the absorbance reflectance of the analyte spots at 238 nm. The method was validated for specificity, linearity, accuracy and precision. Good linearity was achieved in the concentration range 100–800 ng/spot. The RSD of repeatability and intermediate precision were found to be less than 2%, whereas the mean of the recovery data was 100-101%. The detection limit and quantification limit were 22 and 74 ng/spot, respectively. The method is specific, linear, precise, and accurate; it can be used for the routine quality control testing of marketed formulations.Keywords: glimepiride, TLC densitometric, validation of pharmaceutical methods, pharmaceutical analysis, antidiabetic drug Sebuah metode Kromatografi Lapis Tipis (KLT) yang sederhana dan valid telah dikembangkan untuk penentuan glimepiride dalam sediaan tablet. Setelah analit dalam sampel diekstraksi dengan campuran metanol dan amonia 0,2 M (1:1,v/v), ekstrak yang terlihat pada lempeng silika gel F254, yang dikembangkan dengan campuran toluen : metanol : etil asetat (75:20:5, v/v/v). Evaluasi kuantitatif dilakukan dengan mengukur reflektansi absorbansi noda analit pada panjang gelombang 238 nm.Metode ini divalidasi meliputi spesifisitas, linearitas, akurasi dan presisi.Linearitas yang baik dicapai pada rentang konsentrasi 100-800 ng / spot. RSD pengulangan dan presisi intermediate menunjukkan nilai kurang dari 2 %, sedangkan rata-rata data recovery adalah 100-101 % .Batas deteksi dan batas kuantifikasi adalah 22 dan 74 ng / noda.Metode ini spesifik, linear, tepat, dan akurat, bisa digunakan untuk pengujian kontrol kualitas rutin tablet glimepirid dipasarkan. Kata Kunci: glimepiride, TLC densitometric, validation of pharmaceutical methods, pharmaceutical analysis, antidiabetic drug

scholarly journals Tolerance interval testing for assessing accuracy and precision simultaneously

PLoS ONE ◽  
2021 ◽  
Vol 16 (2) ◽  
pp. e0246642
Author(s):  
Chieh Chiang ◽  
Chin-Fu Hsiao
Keyword(s):  
Power Analysis ◽  
Analytical Procedure ◽  
Bivariate Distribution ◽  
Sample Size Determination ◽  
P Value ◽  
Tolerance Interval ◽  
Size Determination ◽  
Tolerance Intervals ◽  
Statistical Inferences ◽  
Accuracy And Precision

Tolerance intervals have been recommended for simultaneously validating both the accuracy and precision of an analytical procedure. However, statistical inferences for the corresponding hypothesis testing are scarce. The aim of this study is to establish a whole statistical inference for tolerance interval testing, including sample size determination, power analysis, and calculation of p-value. More specifically, the proposed method considers the bounds of a tolerance interval as random variables so that a bivariate distribution can be derived. Simulations confirm the theoretical properties of the method. Furthermore, an example is used to illustrate the proposed method.

scholarly journals Controlling bovine brucellosis in the state of São Paulo, Brazil: results after ten years of a vaccination program

2016 ◽  
Vol 37 (5Supl2) ◽  
pp. 3505 ◽  
Author(s):  
Ricardo Augusto Dias ◽  
Ana Paula Cunha Belchior ◽  
Rodrigo De Souza Ferreira ◽  
Rita Coelho Gonçalves ◽  
Ricardo Souza Costa Barão de Aguiar ◽  
...  
Keyword(s):  
Confidence Interval ◽  
Sao Paulo ◽  
The State ◽  
Vaccination Program ◽  
São Paulo ◽  
Bovine Brucellosis ◽  
Paulo State ◽  
Significant Difference ◽  
Strain Vaccine ◽  
São Paulo State

A cross- sectional study was carried out, between May and November 2011, to estimate the situation of the bovine brucellosis in São Paulo State, 10 years after the commencement of the vaccination of the heifers with the S19 strain. The State was divided into seven regions and in each of them, 300 farms with reproductive activity were randomly chosen and considered as primary sample units. A fixed number of cows was randomly selected and tested for antibodies against Brucella spp. A farm was considered infected if at least one female tested positive. In the selected farms, an epidemiological questionnaire was administered which focused on herd traits as well as husbandry and sanitary practices that could be associated with the risk of infection. The prevalence (percentile, [95% confidence interval]) of infected herds was 10.2% [8.8-11.8] for the State, and for the regions, it varied from 7.3% [4.7-11.2] to 12.3% [8.8-16.8], not showing significant difference between different regions. The apparent prevalence of positive farms in the State and regions remained similar to the prevalence observed 10 years before. The prevalence of positive animals was 2.4% [1.8-3.1] in the State and varied from 1.1% [0.6-2] to 3.5% [1.7-7.1] in the regions, not showing significant difference between regions. Again, there was no difference in the prevalence of positive animals after 10 years of the vaccination program. The risk factors (odds ratio, 95% confidence interval) associated with bovine brucellosis in the State included number of cows ? 24 (3.08, 2.22-4.27) and the acquisition of breeding animals (1.33, 0.95-1.87). The São Paulo State should conduct systematic vaccination coverage of above 80% of the eligible heifers with the S19 strain vaccine annually. Moreover, the State should emphatically use RB51 strain vaccine in females above 8 months of age not vaccinated with S19 strain vaccine. An efficient animal health education program to orientate farmers to test replacement animals for brucellosis prior to introduction in their herds should also be implemented.

scholarly journals Effect of Turbulent-Flow Pasteurization on Survival of Mycobacterium avium subsp.paratuberculosis Added to Raw Milk

2001 ◽  
Vol 67 (9) ◽  
pp. 3964-3969 ◽  
Author(s):  
Lindsay E. Pearce ◽  
H. Tuan Truong ◽  
Robert A. Crawford ◽  
Gary F. Yates ◽  
Sonia Cavaignac ◽  
...  
Keyword(s):  
Confidence Interval ◽  
Turbulent Flow ◽  
Mycobacterium Avium ◽  
Culture Method ◽  
Egg Yolk ◽  
Raw Milk ◽  
Pilot Scale ◽  
Heat Sensitivity ◽  
Decimal Reduction Time ◽  
The Mean

ABSTRACT A pilot-scale pasteurizer operating under validated turbulent flow (Reynolds number, 11,050) was used to study the heat sensitivity ofMycobacterium avium subsp.paratuberculosis added to raw milk. The ATCC 19698 type strain, ATCC 43015 (Linda, human isolate), and three bovine isolates were heated in raw whole milk for 15 s at 63, 66, 69, and 72°C in duplicate trials. No strains survived at 72°C for 15 s; and only one strain survived at 69°C. Means of pooled Dvalues (decimal reduction times) at 63 and 66°C were 15.0 ± 2.8 s (95% confidence interval) and 5.9 ± 0.7 s (95% confidence interval), respectively. The mean extrapolatedD 72°C was <2.03 s. This was equivalent to a >7 log10 kill at 72°C for 15 s (95% confidence interval). The mean Z value (degrees required for the decimal reduction time to traverse one log cycle) was 8.6°C. These five strains showed similar survival whether recovery was on Herrold's egg yolk medium containing mycobactin or by a radiometric culture method (BACTEC). Milk was inoculated with fresh fecal material from a high-level fecal shedder with clinical Johne's disease. After heating at 72°C for 15 s, the minimum M. avium subsp.paratuberculosis kill was >4 log10. Properly maintained and operated equipment should ensure the absence of viable M. avium subsp. paratuberculosisin retail milk and other pasteurized dairy products. An additional safeguard is the widespread commercial practice of pasteurizing 1.5 to 2° above 72°C.

scholarly journals Development and validation of analytical methodology with focus on the qualification of powder mixers

2015 ◽  
Vol 51 (2) ◽  
pp. 273-284 ◽  
Author(s):  
Pedro de Freitas Fiorante ◽  
Rodrigo Dias Martins ◽  
Mauri Sergio Alves Palma
Keyword(s):  
Hydrochloric Acid ◽  
Ferric Oxide ◽  
Analytical Procedure ◽  
Maximum Deviation ◽  
Hydrochloric Acid Concentration ◽  
Intermediate Precision ◽  
Analytical Methodology ◽  
Relative Standard ◽  
Performance Qualification ◽  
The Stability

<p>This study aims at developing an analytical procedure capable of quantifying the ferric oxide present in the mixture of ferric oxide/lactose monohydrate (0.4% w/w). The analytical procedure was checked for specificity, linearity, precision (system repeatability, procedure repeatability and intermediate precision), accuracy, stability of solutions and robustness of the procedure. The concentration of Fe (III) was determined by spectrophotometry at 480 nm based on calibration curves. The specificity was verified. The linearity was obtained in the range of 11.2 to 16.8 µg of ferric oxide/mL. The relative standard deviation (RSD) of the system repeatability, procedure repeatability and intermediate precision, were not more than 2%. The RSD of the accuracy values were less than 0.75%. The stability of the samples was checked over a 24 hours assay. In the robustness evaluation, the wavelength and the concentration of hydrochloric acid varied. The maximum absorbance deviation due to wavelength variation was 0.14 percent, and the maximum deviation due to the hydrochloric acid concentration variation was 2.4%, indicating that the concentration of hydrochloric acid is critical to the analysis of ferric oxide. The procedure developed was validated and is suitable to the performance qualification of powder mixers.</p>

scholarly journals Changes in spending and service use after a state autism insurance mandate

Autism ◽  
2017 ◽  
Vol 23 (1) ◽  
pp. 167-174 ◽  
Author(s):  
Brendan Saloner ◽  
Colleen L Barry
Keyword(s):  
Autism Spectrum Disorder ◽  
Confidence Interval ◽  
Health Plan ◽  
Service Use ◽  
Autism Spectrum ◽  
Employee Health ◽  
The State ◽  
Spectrum Disorder ◽  
Disorder Treatment ◽  
State Employee

Almost all states have insurance coverage mandates for childhood autism spectrum disorder treatment, yet little is known about how mandates affect spending and service use. We evaluated a 2011 Kansas law mandating comprehensive coverage of autism spectrum disorder treatments in the State Employee Health Plan. Data were extracted from the Kansas All-Payer Claims Database from 2009 to 2013 for enrollees of State Employee Health Plan and private health plans. The sample included children aged 0–18 years with >2 claims with an autism spectrum disorder diagnosis insured through State Employee Health Plan or a comparison group enrolled through private health plans. We estimated differences-in-differences regression models to compare trends among State Employee Health Plan to privately insured children. Average annual total spending on autism spectrum disorder services increased by US$912 (95% confidence interval: US$331–US$1492) and average annual out-of-pocket spending on autism spectrum disorder services increased by US$138 (95% confidence interval: US$53–US$223) among diagnosed children in the State Employee Health Plan relative to the comparison group following the mandate, representing 92% and 75% increases over baseline total and out-of-pocket autism spectrum disorder spending, respectively. Average annual quantity of outpatient autism spectrum disorder services increased by 15.0 services (95% confidence interval: 8.4–21.6) among children in the State Employee Health Plan, more than doubling the baseline average. Implementation of a comprehensive autism spectrum disorder mandate in the Kansas State Employee Health Plan was associated with substantial increases in service use and spending for autism spectrum disorder treatment among autism spectrum disorder–diagnosed children.

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