scholarly journals Microbiological Antibiotic Assay Validation of Gentamicin Sulfate Using Two-Dose Parallel Line Model (PLM)

2021 ◽  
Vol 2 (4) ◽  
pp. 306-319
Author(s):  
Mostafa Essam Eissa ◽  
Engy Refaat Rashed ◽  
Dalia Essam Eissa
Keyword(s):  
Aminoglycoside Antibiotic ◽  
Parallel Line ◽  
Control Analysis ◽  
Line Model ◽  
Gentamicin Sulfate ◽  
Accuracy And Precision ◽  
Assay Design ◽  
Diffusion Assay ◽  
Digital Caliper

Till nowadays microbiological assay is still widely used with several antibiotics that are composed of a mixture of related active compounds. However, obtaining a reasonably valid determination of the potency is dependent on the validity and the suitability of the assay design. The present work aimed to validate an assay design of an aminoglycoside antibiotic (Gentamicin Sulfate) using a two-dose Parallel Line Model agar diffusion assay in a large 8×8 rectangular plate. All preparatory procedures were done following United States Pharmacopeia and the Inhibition Zones were measured using a digital caliper to the nearest 0.01 mm. Analysis of variance of compendial requirements of regression and parallelism were found to be satisfactorily meeting the acceptance criteria. Specificity was achieved for the product under investigation with no detectable IZ that could be found for all components except the antibiotic. The validation method showed acceptable linearity of r2≥0.98. Accuracy and precision parameters showed RSD (%)<2. All relative error value estimates were below 4%. The proposed validation design for 32×32 cm antibiotic plates yielded valid results and can be projected for the routine Quality Control analysis of the antibiotic material, especially which is incorporated into a finished medicinal dosage form. Doi: 10.28991/HIJ-2021-02-04-04 Full Text: PDF

Quantitative determination of antibiotics by automated six-point parallel-line agar diffusion assay

1974 ◽  
Vol 40 (4) ◽  
pp. 610-611 ◽  
Author(s):  
D. A. Detmar ◽  
K. H. F. van Hemert ◽  
R. Malherbe ◽  
J. G. Oostendorp
Keyword(s):  
Quantitative Determination ◽  
Parallel Line ◽  
Agar Diffusion ◽  
Agar Diffusion Assay ◽  
Diffusion Assay

scholarly journals Simultaneous RP HPLC Determination of Aceclofenac, Paracetamol and Tizanidine in Pharmaceutical Preparations

2010 ◽  
Vol 7 (1) ◽  
pp. 260-264 ◽  
Author(s):  
V. V. Vaidya ◽  
G. R. Singh ◽  
M. P. Choukekar ◽  
M. B. Kekare
Keyword(s):  
High Performance ◽  
Pharmaceutical Preparations ◽  
High Performance Liquid Chromatographic ◽  
Control Analysis ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A simple, fast and precise reverse phase high performance liquid chromatographic method is developed for the simultaneous determination of aceclofenac, paracetamol and tizanidine. Chromatographic separation of the three drugs were performed on a hypersil C18column (250 mm x 4.6 mm, 5 µm) as stationary phase with a mobile phase comprising of mix phosphate buffer pH 7.0: acetonitrile (40:60 v/v), at a flow rate of 0.7 mL min-1and UV detection at 230 nm. The proposed method was validated for linearity, accuracy, precision, LOD, LOQ. Linearity, accuracy and precision were found to be acceptable over the ranges of 100-300 µg mL-1for aceclofenac, 500-1500 µg mL-1for paracetamol and 2-6 µg mL-1for tizanidine HCl equivalent to tizanidine. It can be conveniently adopted for routine quality control analysis.

Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

Recent Applications of High Performance Thin Layer Chromatography and Derivative Spectrophotometry in Pharmaceutical Analysis

2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Pharmaceutical Analysis ◽  
High Performance ◽  
Degradation Products ◽  
Derivative Spectrophotometry ◽  
Accuracy And Precision ◽  
Post Marketing ◽  
Layer Chromatography

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.

Simultaneous Determination of Six Components in Jingzhiguanxin Tablet by High-Performance Liquid Chromatography

2019 ◽  
Vol 15 (2) ◽  
pp. 130-137
Author(s):  
Hui Jiang ◽  
Lianhao Fu ◽  
Yu Wang ◽  
Shaozhi Wang ◽  
Xiaoxu Zhang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Tanshinone Iia ◽  
Array Detector ◽  
Control Analysis ◽  
Active Components ◽  
Quality Control Analysis

Background: Jingzhiguanxin (JZGX) tablet, a traditional Chinese prescription, is commonly used for treating coronary heart disease and angina pectoris in the clinic. There are six active components (Danshensu (DSS), Protocatechuic aldehyde (PD), Paeoniflorin (PF), Ferulic acid (FA), Salvianolic acid B (Sal B) and Tanshinone IIA (TA)) in JZGX tablet. </P><P> Objective: In this paper, a simple and reliable method was used for simultaneous determining the six active components by high-performance liquid chromatography coupled with diode array detector (HPLC-DAD). Methods: These six active components were separated on an Agilent Zorbax Eclipse XDB-C18 column (150 mmx4.6 mm, 5 µm) at 30 °C. Acetonitrile (A), methanol (B) and 0.5% H3PO4 aqueous solution (C) were used as mobile phase for gradient elution. The flow rate was 1 mL/min and the detection wavelengths were set at 280 nm for DSS, PD and Sal B, 230 nm for PF, 320 nm for FA and 270 nm for TA, respectively. Results: All of the six components showed good linearity regressions (r2≥0.9997) in the detected concentration range. The recovery rates and coefficient of variation (CV) for all analytes were 98.66%- 100.18% and 0.75%-1.89%, respectively. This method was successfully applied to simultaneously determine the six components in JZGX tablet from different batches and manufacturers. Conclusion: The validated method can be used in routine quality control analysis of JZGX tablet without any interference.

A Green Liquid Chromatographic Method For The Simultaneous Determination of Chlorpheniramine Maleate, Pseudoephedrine Hydrochloride and Propyphenazone

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Green Analytical Chemistry ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.

A Rapid Method for Determination of Buprenorphine and Norbuprenorphine in Urine by UPLC-MS/MS

2020 ◽  
Vol 16 ◽  
Author(s):  
Aykut Kul ◽  
Murat Ozdemir ◽  
Selma Ozilhan ◽  
Olcay Sagirli
Keyword(s):  
Forensic Science ◽  
Rapid Method ◽  
Proficiency Testing ◽  
Mass Spectrometer ◽  
Illicit Market ◽  
Analysis Methods ◽  
Accuracy And Precision ◽  
Lower Limits

Background: Buprenorphine is quite common in the illicit market. Buprenorphine-containing drugs abuse is frequently encountered in patients. The analysis methods used to determine the abuse of buprenorphine and norbuprenorphine are important for forensic science. Buprenorphine is metabolized to norbuprenorphine by the liver. Objective: Therefore, the determination of buprenorphine and norbuprenorphine in urine is one of the methods to determine the abuse of buprenorphine. Methods: In this study, we have developed a precise, simple, and rapid ultra-performance liquid chromatographytandem mass spectrometer method for the determination of buprenorphine and norbuprenorphine simultaneously. Results: The developed method was validated in terms of selectivity and linearity, which was in the range of 9–1800 ng/mL for both buprenorphine and norbuprenorphine. The intra-assay and inter-assay accuracy and precision were found within acceptable limits of the EMA guideline. Lower limits of quantitation were 9 ng/mL for both buprenorphine and norbuprenorphine. Conclusion: The developed method was successfully applied for the determination of both analytes in the proficiency testing samples.

scholarly journals Simplified and Rapid Determination of Primaquine and 5,6-Orthoquinone Primaquine by UHPLC-MS/MS: Its Application to a Pharmacokinetic Study

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Rapid Determination ◽  
Active Metabolites ◽  
Chromatography Tandem Mass Spectrometry ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Isocratic Mode

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.

Comparative Study for the Assay of Plant Derived Chemicals in Pharmaceutical Formulation Using Methods Dependent on Factorized Spectra

2021 ◽  
Author(s):  
Nesma M Fahmy ◽  
Adel M Michael
Keyword(s):  
Pharmaceutical Formulations ◽  
Pharmaceutical Formulation ◽  
Ternary Mixtures ◽  
Ratio Method ◽  
The Novel ◽  
Naturally Occurring ◽  
Accuracy And Precision ◽  
Validation Parameters ◽  
Significant Difference

Abstract Background Modern built-in spectrophotometer software supporting mathematical processes provided a solution for increasing selectivity for multicomponent mixtures. Objective Simultaneous spectrophotometric determination of the three naturally occurring antioxidants—rutin(RUT), hesperidin(HES), and ascorbic acid(ASC)—in bulk forms and combined pharmaceutical formulation. Method This was achieved by factorized zero order method (FZM), factorized derivative method (FD1M), and factorized derivative ratio method (FDRM), coupled with spectrum subtraction(SS). Results Mathematical filtration techniques allowed each component to be obtained separately in either its zero, first, or derivative ratio form, allowing the resolution of spectra typical to the pure components present in Vitamin C Forte® tablets. The proposed methods were applied over a concentration range of 2–50, 2–30, and 10–100 µg/mL for RUT, HES, and ASC, respectively. Conclusions Recent methods for the analysis of binary mixtures, FZM and FD1M, were successfully applied for the analysis of ternary mixtures and compared to the novel FDRM. All were revealed to be specific and sensitive with successful application on pharmaceutical formulations. Validation parameters were evaluated in accordance with the International Conference on Harmonization guidelines. Statistical results were satisfactory, revealing no significant difference regarding accuracy and precision. Highlights Factorized methods enabled the resolution of spectra identical to those of pure drugs present in mixtures. Overlapped spectra of ternary mixtures could be resolved by spectrum subtraction coupled FDRM (SS-FDRM) or by successive application of FZM and FD1M.

scholarly journals Spectrophotometric determination of dothiepin hydrochloride in pharmaceuticals through ion-pair complexation reaction

2012 ◽  
Vol 18 (2) ◽  
pp. 339-347 ◽  
Author(s):  
Sameer Abdulrahman ◽  
Kanakapura Basavaiah
Keyword(s):  
Ion Pair ◽  
Pure Form ◽  
Bromocresol Green ◽  
Bromophenol Blue ◽  
Complexation Reaction ◽  
Conditional Stability ◽  
Conditional Stability Constant ◽  
Accuracy And Precision ◽  
Significant Difference

Two simple, sensitive and extraction-free spectrophotometric methods are described for the determination of dothiepin hydrochloride (DOTH) both in pure form and in pharmaceutical tablets. The methods are based on ion-pair complex formation between dothiepin base (DOT) and two acidic dyes, namely, bromophenol blue (BPB) or bromocresol green (BCG) with absorption maximum at 425 nm for BPB method or 430 nm for BCG method. Beer?s law is obeyed over the concentration ranges of 1.0-15.0 and 1.0-17.5 ?g mL-1 DOT for BPB and BCG methods, respectively. The molar absorptivity values and Sandell?s sensitivity values are reported for both methods. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.18 and 0.53 ?g mL-1 for BPB method, and 0.17 and 0.50 ?g mL-1 for BCG method, respectively. The stoichiometry of the complex in either case was found to be 1: 1 and the conditional stability constant (KF) of the complexes has also been calculated. The proposed methods were applied successfully to the determination of DOTH in pure form and in its tablet form with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and variance ratio F-test at 95% confidence level and there was no significant difference between the official and proposed methods with regard to accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition technique.

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