Bioanalysis - Method Development, Validation, Sample Preparation, its Detection Techniques and its Application

2021 ◽  
pp. 297-305
Author(s):  
Seema R. Nikam ◽  
Amol S. Jagdale ◽  
Sahebrao S. Boraste ◽  
Shrikant B Patil
Keyword(s):  
Sample Preparation ◽  
Method Development ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Bioequivalence Study ◽  
Time Frame ◽  
Biological Drugs ◽  
Detection Techniques ◽  
Validation Parameters ◽  
Limit Of Quantitation

Quantitatively measurements of chemical and biological drugs and their metabolites in the biological sample. This used in clinical and non-clinical studies. Non clinical including Pharmacokinetic and Toxic kinetic study, and clinical including Bioavailability, Bioequivalence study. This are play significant role and help in improvement in technology and analytical methods. Recent years have witnessed the introduction of several high- quality review articles into the literature covering various scientific and technical aspects of bioanalysis. Method validation and development use for the purpose of suitability of method for their intended purpose, this are important in Drug Discovery and Development. It including a validation parameters are Accuracy, Precision, Range, Calibration Curve, Recovery, Limit of Detection, Limit of Quantitation, Specificity, Selectivity and Stability, Ruggedness. This applicable in bio analysis, FDA and EMA guidelines. There are 3 main Extraction techniques used in sample preparation in bioanalysis is precipitation, liquid –liquid extraction, solid phase extraction. Detection of analyte by using hyphenated and chromatographic techniques like LC-MS/MS, HPLC, GC-MS. This LC-MS/MS is commonly used in a bioanalysis. This bio analysis study used in Pharmaceutical, Biomedical research purpose. Many challenges in pharmaceutical industry that fulfill by the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality.

scholarly journals THE RAPID AND GREEN HAIR ANALYSIS METHOD DEVELOPMENT USING FTIR FOR PAPAVERINE HCL DETERMINATION

2019 ◽  
pp. 211-217 ◽  
Author(s):  
ILMA NUGRAHANI ◽  
STEPHANIE SULISTIANA ◽  
SLAMET IBRAHIM
Keyword(s):  
Hair Sample ◽  
Method Development ◽  
Limit Of Detection ◽  
Area Under The Curve ◽  
Forensic Analysis ◽  
Percent Recovery ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Papaverine Hydrochloride

Objective: This study was aimed to develop a rapid analysis using FTIR (Fourier Transform Infra-Red) for papaverine hydrochloride (HCl) determination in the hair sample, supported by a mathematically manipulation; which never been reported before in toxicology and forensic analysis. Methods: Firstly, the method was checked its validity to ensure the feasibility for the quantitative purpose. The absorbance spectrums were collected by measure the drug, matrix, and its mixture. A spectra which showed the best specificity and linearity then was selected and derived. Afterwards, the area under the curve (AUC) was measured. A series of concentration was used for compose the calibration curve. Based on the result, some validation parameters were checked thoroughly. Further, for sample preparation, hair was collected non-invasively, then was decontaminated using soap. Next, it was immersed into a papaverine HCl solution at a concentration of 25 mg/ml along days. Finally, the amount of drugs absorbed were measured by the developed method using FTIR. Results: Experimental data showed that all validation parameters could be fulfilled by the developed method. The selected spectra for the content determination was 1320-1230 cm-1. Its linearity was represented by a correlation coefficient value (r) ≥ 0.9999, variation coefficient (Vxo) ≤ 2.0%. The limit of detection (LOD) was 0.00618% w/w, meanwhile, the limit of quantitation (LOQ) was 0.02060% w/w, respectively. The percent recovery was in the range 97-103% with the relative standard deviation (RSD) was ≤ 2.0%. The drug has detected after 72 h immersion, moreover, after 192 h the concentration gained was 0.1594±0.0011% w/w. Conclusion: As the conclusion, FTIR absorbance-derivative method is adequate as a rapid procedure for determine papaverine HCl in the hair sample. This method shows the appropriate of specificity, accuracy and precise. In addition, it shows the advantages of simplicity, green/eco-friendlier, and cost-efficiency.

scholarly journals Analytical method development and validation studies for the estimation of H2 receptor antagonist drug (Ranitidine)

2021 ◽  
Vol 7 (2) ◽  
pp. 85
Author(s):  
Renuka Manjunath ◽  
Deepak Kumar Jha
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
H2 Receptor Antagonist ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

<p class="abstract"><strong>Background:</strong> An analytical science in the development, finding a new molecules and procreation of pharmaceuticals has been an extensive approached. From the evaluation over small quantities of complex biological substances to the quality monitoring of the finished dosage form, the use on analytical technology know- how covers an ample thoroughness over techniques or disciplines.</p><p class="abstract"><strong>Methods:</strong> Reversed phase high performance liquid chromatography (RP-HPLC) approach has been promoted for the discernment over Ranitidine (RAN) within pharmaceutical dosage form split of RAN was accomplished inside a unaccompanied chromatographic run of an Phenomenix column size 5 μm 4.6x250 mm along with UV analysis at 227 nm wavelength, below isocratic conditions, using Ammonium acetate and Methanol (pH 6.0) in 80:20 ratio. Validation parameters had been observed in accordance with exhibit linearity, accuracy, precision, Limit of Quantitation and Limit of detection in conformity in imitation of ICH guidelines.  </p><p class="abstract"><strong>Results:</strong> The contemporary approached demonstrates significant linearity upon the range concerning 50-202.5 μg/ml for RAN followed by intra-day and inter-day precision, expressed so the relative standard deviation (RSD), on replicates is &lt;2.0 and accuracy among the range over 98-102%.</p><p class="abstract"><strong>Conclusions:</strong> The flourished RP-HPLC technique was once innovative, suitable for detecting RAN in pure form and in pharmaceutical preparation.</p>

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Triethyl orthoformate content) in 5-methyl-4-isoxazole carboxylic acid (5-MIA) by using GC Technique

2021 ◽  
Vol 37 (2) ◽  
pp. 348-353
Author(s):  
Mohan bhatale ◽  
Neelakandan kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan ramalingam
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Fused Silica ◽  
Triethyl Orthoformate ◽  
Concentration Limit ◽  
Simultaneous Estimation ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Development And Validation

A simple, selective, precise and accurate Gas chromatographic method for determination of Triethyl orthoformate content (Genotoxic impurity) in 5-MIA is reported. The GC method development and validation as per the International Council for Harmonisation (ICH) guidelines Q2(R1). The effective chromatographic separations were achieved on DB-624, 60 m × 0.53 mm ID, with film thickness of 3.0 μm (Fused silica capillary column), Capillary injector temperature of 150°C, and Nitrogen Carrier gas. This method is unique as there is no UV response; hence GC Method was developed for Triethyl orthoformate. The elution was accomplished with the flow rate of 5.0 mL/min and Split Flow of 10 mL/minute. Detection was performed with FID detector (temp. 260°C) and with column oven temperature program. Methods range from limit of quantitation (LOQ) to 150% level with respect to specification concentration limit of impurity is linear and correlation coefficient of impurity is > 0.99. The linearity of Triethyl orthoformate covered from LOQ to 113 ppm (ie. LOQ to 150% of specification limit) and LOQ to 19 ppm wrt standard concentration. The limit of detection (LOD)values were observed were 2.5 ppm and limit of quantitation (LOQ) were 7.7 ppm, respectively. The parameters selected for the method validated were from international conference on harmonization guidelines, Indian pharmacopeia, USP. The percentage recovery from LOQ, 50% ,100% to 150% level of content were 87.70%, 98.60%, 102.25 and 96.59% respectively. The %RSD values were for LOQ to 150% were from 1.64%, 0.89%, 1.78 % and 1.49%. The range was covered from LOQ to 150% of standard concentration. The results of validation parameters were found in the acceptance range. Standard and sample were stable up to 30 h at when stored at room temperature. Also it was quite robust for the small change in method parameter like, change in column oven temperature(± 5 degree). Hence from the above parameter it was concluded that the GC method with FID detector is selective, precise, linear, and robust for simultaneous estimation of Triethyl orthoformate in Drug Substances.

scholarly journals ESTIMATION OF CELECOXIB IN HUMAN PLASMA BY RAPID AND SELECTIVE LC-MS/MS METHOD FOR A BIOEQUIVALENCE STUDY

2018 ◽  
Vol 10 (10) ◽  
pp. 16 ◽  
Author(s):  
Nirav P. Patel ◽  
Mallika Sanyal ◽  
Pranav S. Shrivastav ◽  
Bhavin N. Patel
Keyword(s):  
Human Plasma ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Study Data ◽  
Acetate Solution ◽  
Limit Of Quantitation ◽  
Negative Ionization

Objective: A selective, sensitive and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been developed for the determination of celecoxib (CXB) in negative ionization mode.Methods: Celecoxib and celecoxib-D7 (CXB-D7) as internal standard (IS) were extracted from 300 µl human plasma by solid-phase extraction using strata-X SPE cartridges. Chromatographic separation was achieved on ACE C8-300 (50 × 4.0 mm, 3.0 μm) column using methanol-1.0 mmol ammonium acetate solution in 80:20 (v/v) ratio. The protonated precursor to product ion transitions studied for CXB and CXB-D7 were m/z 380.0 → 315.9 and 387.0 → 323.0, respectively.Results: The limit of detection (LOD) and lower limit of quantitation of the method were 2.50 and 10.0 ng/ml respectively with a linear dynamic range of 10.0-4000 ng/ml for CXB. The intra-batch and inter-batch precision (% CV) and mean relative recovery across quality control levels is<7.2 % and 85.5 % respectively. Matrix effect in human plasma, expressed as IS-normalized matrix factor ranged from 0.99-1.03.Conclusion: The method was successfully applied in healthy subjects using a single dose of 400 mg celecoxib capsules under fasting and fed conditions. The reproducibility in the measurement of study data is demonstrated by incurred sample reanalysis.

scholarly journals Measurement of HDO Products Using GC-TCD: Towards Obtaining Reliable Analytical Data

2018 ◽  
Vol 5 (1) ◽  
pp. 1-11 ◽  
Author(s):  
Oman Zuas ◽  
Harry Budiman ◽  
Dieni Mansur ◽  
Muhammad Rizky Mulyana
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Analytical Data ◽  
Sample Treatment ◽  
Gaseous Products ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

Abstract This paper reported the method development and validation of a gas chromatography with thermal conductivity detector (GC-TCD) method for the measurement of the gaseous products of hydrodeoxygenation (HDO). The method validation parameters include selectivity, precision (repeatability and reproducibility), accuracy, linearity, limit of detection (LoD), limit of quantitation (LoQ), and robustness. The results showed that the developed method was able to separate the target components (H2, CO2, CH4 and CO) from their mixtures without any special sample treatment. The validated method was selective, precise, accurate, and robust. Application of the developed and validated GC-TCD method to the measurement of by-product components of HDO of bio-oil revealed a good performance with relative standard deviation (RSD) less than 1.0% for all target components, implying that the process of method development and validation provides a trustworthy way of obtaining reliable analytical data.

scholarly journals A REVIEW ON ANALYTICAL METHOD DEVELOPMENT AND VALIDATION

2018 ◽  
Vol 10 (6) ◽  
pp. 8 ◽  
Author(s):  
Shivani Sharma ◽  
Swapnil Goyal ◽  
Kalindi Chauhan
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Good Manufacturing Practice ◽  
Raw Material ◽  
Analytical Technique ◽  
Effective Manner ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Development And Validation

The top objective of any pharmaceutical industry is to produce products of necessary characteristic and quality reliably, in a cost-effective manner. Development of a method is essential for discovery, development, and evaluation of medicines in the pharmaceutical formulation. The main aim of this review article was to check the development and validation of the procedure employed for the medication from the starting of the formulation to the complete commercial batch of product. At the point when an analytical technique is applied to produce outcomes for the quality of medicine associated samples, it is necessary that the outcomes are reliable. In the pharma industry, validation policy is documented for how to perform validation, types of validation and validation policy are complied with the necessities of good manufacturing practice (GMP) regulations. Validation is very important for the effective running of the pharmaceutical firms. At every stage from raw material to the finished, stability, everywhere validation was performed. The method was developed properly, and validation parameters are explained in terms of accuracy, specificity, precision, limit of detection (LOD), limit of quantitation (LOQ), ruggedness, robustness, and system suitability testing with the example of certain drugs. All validation parameters are used in the routine and stability analysis.

Recent Trends in the Development of Green Microextraction Techniques for the Determination of Hazardous Organic Compounds in Wine

2019 ◽  
Vol 15 (7) ◽  
pp. 788-800 ◽  
Author(s):  
Natasa P. Kalogiouri ◽  
Victoria F. Samanidou
Keyword(s):  
Sample Preparation ◽  
Solid Phase Extraction ◽  
Organic Compounds ◽  
Method Development ◽  
Solid Phase ◽  
Stir Bar Sorptive Extraction ◽  
Phase Extraction ◽  
Microextraction Techniques ◽  
Hazardous Organic Compounds

Background:The sample preparation is the most crucial step in the analytical method development. Taking this into account, it is easily understood why the domain of sample preparation prior to detection is rapidly developing. Following the modern trends towards the automation, miniaturization, simplification and minimization of organic solvents and sample volumes, green microextraction techniques witness rapid growth in the field of food quality and safety. In a globalized market, it is essential to face the consumers need and develop analytical methods that guarantee the quality of food products and beverages. The strive for the accurate determination of organic hazards in a famous and appreciated alcoholic beverage like wine has necessitated the development of microextraction techniques.Objective:The objective of this review is to summarize all the recent microextraction methodologies, including solid phase extraction (SPE), solid phase microextraction (SPME), liquid-phase microextraction (LPME), dispersive liquid-liquid microextraction (DLLME), stir bar sorptive extraction (SBSE), matrix solid-phase dispersion (MSPD), single-drop microextraction (SDME) and dispersive solid phase extraction (DSPE) that were developed for the determination of hazardous organic compounds (pesticides, mycotoxins, colorants, biogenic amines, off-flavors) in wine. The analytical performance of the techniques is evaluated and their advantages and limitations are discussed.Conclusion:An extensive investigation of these techniques remains vital through the development of novel strategies and the implication of new materials that could upgrade the selectivity for the extraction of target analytes.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

scholarly journals Sample Preparation and Extraction in Small Sample Volumes Suitable for Pediatric Clinical Studies: Challenges, Advances, and Experiences of a Bioanalytical HPLC-MS/MS Method Validation Using Enalapril and Enalaprilat

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
Bjoern B. Burckhardt ◽  
Stephanie Laeer
Keyword(s):  
Sample Preparation ◽  
Solid Phase Extraction ◽  
Method Development ◽  
Matrix Effects ◽  
Solid Phase ◽  
Scale Up ◽  
Small Sample ◽  
Positive Pressure ◽  
Phase Extraction ◽  
Bioanalytical Method

In USA and Europe, medicines agencies force the development of child-appropriate medications and intend to increase the availability of information on the pediatric use. This asks for bioanalytical methods which are able to deal with small sample volumes as the trial-related blood lost is very restricted in children. Broadly used HPLC-MS/MS, being able to cope with small volumes, is susceptible to matrix effects. The latter restrains the precise drug quantification through, for example, causing signal suppression. Sophisticated sample preparation and purification utilizing solid-phase extraction was applied to reduce and control matrix effects. A scale-up from vacuum manifold to positive pressure manifold was conducted to meet the demands of high-throughput within a clinical setting. Faced challenges, advances, and experiences in solid-phase extraction are exemplarily presented on the basis of the bioanalytical method development and validation of low-volume samples (50 μL serum). Enalapril, enalaprilat, and benazepril served as sample drugs. The applied sample preparation and extraction successfully reduced the absolute and relative matrix effect to comply with international guidelines. Recoveries ranged from 77 to 104% for enalapril and from 93 to 118% for enalaprilat. The bioanalytical method comprising sample extraction by solid-phase extraction was fully validated according to FDA and EMA bioanalytical guidelines and was used in a Phase I study in 24 volunteers.

Method of Validation for Residual Solvents in Bisoprolol Fumarate by GC Technique

2021 ◽  
pp. 147-155
Author(s):  
Sandip A Telavane ◽  
Seema Kothari ◽  
Manohar V. Lokhande
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Technique ◽  
Range Limit ◽  
Column Temperature ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Chromatographic Condition ◽  
Methylene Dichloride

Validation is important technique for detection, progress and estimation of drugs for pharmaceutical analysis. Aim of this article was to check the progress and validation of the method employed for the Residual Solvents in Bisoprolol Fumarate by Gas Chromatographic technique. The objective of this protocol is to validate a GC method of analysis for detection and Quantification of Residual Solvents Methanol, Acetone and Methylene dichloride in Bisoprolol Fumarate. In the pharmaceutical industry, validation policy is more important for documented of validation, types of validation and validation policy. The method was developed accurately and validation parameters are explained. Chromatographic condition was GC- 2014, gas chromatograph equipped with FID detector, column: 30 m x 0.32 mm ID x 1.8 µm DB - 624 capillary column or equivalent and column temperature was 45°C (hold 7 minutes) to 250°C @ 40°C/minutes, hold at 250°C for 3 minutes. The parameters such as Accuracy, Specificity, Precision, Linearity and Range, Limit of detection (LOD), Limit of quantitation (LOQ), ruggedness, robustness and system suitability testing with residual solvent such as Methanol, Acetone and methylene dichloride. All validation parameters are used in the routine and stability analysis.

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