scholarly journals Development and Validation of a GC-MS Method for the Detection and Quantification of Clotiapine in Blood and Urine Specimens and Application to a Postmortem Case

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Giulio Mannocchi ◽  
Flaminia Pantano ◽  
Roberta Tittarelli ◽  
Miriam Catanese ◽  
Federica Umani Ronchi ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Internal Standard ◽  
Urine Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Published Data ◽  
Limit Of Quantification ◽  
Blood And Urine Samples ◽  
Development And Validation ◽  
Urine Specimens ◽  
Detection And Quantification

Introduction. Clotiapine is an atypical antipsychotic of the dibenzothiazepine class introduced in a few European countries since 1970, efficient in treatment-resistant schizophrenic patients. There is little published data on the therapeutic and toxic concentrations of this drug.Aims. The aim of the present study is the development and validation of a method that allows the detection and quantification of clotiapine in blood and urine specimens by gas chromatography-mass spectrometry (GC-MS).Methods. Validation was performed working on spiked postmortem blood and urine samples. Samples were extracted with liquid-liquid extraction (LLE) technique at pH 8.5 with n-hexane/dichloromethane (85/15 v/v) and analysis was followed by GC-MS. Methadone-d9 was used as internal standard.Results. The limit of detection (LOD) was 1.2 and 1.3 ng/mL for urine and blood, respectively, while the lower limit of quantification (LLOQ) was 3.9 and 4.3 ng/mL, respectively. Linearity, precision, selectivity, accuracy, and recovery were also determined. The method was applied to a postmortem case. The blood and urine clotiapine concentrations were 1.32 and 0.49 μg/mL, respectively.Conclusions. A reliable GC-MS method for the detection and quantification of clotiapine in blood and urine samples has been developed and fully validated and then applied to a postmortem case.

Development and Validation of a Quantitative NMR Method for the Determination of the Commercial Tablet Formulation of Sulfasalazine

2018 ◽  
Vol 15 (1) ◽  
pp. 39-44 ◽  
Author(s):  
Feng Su ◽  
Zi-qing Sun ◽  
Xian-rui Liang
Keyword(s):  
Maleic Acid ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Tablet Formulation ◽  
Quantitative Nmr ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Development And Validation ◽  
Good Agreement

Introduction: Quantitative NMR spectroscopy (qNMR) is a rapid, simple and efficient method for the assay of sulfasalazine (SSZ) in commercial tablet formulation. Materials and Methods: The qNMR method was demonstrated using maleic acid as an internal standard and DMSO-d6 as a solvent. The characteristic signals of SSZ at δ 8.36 ppm and maleic acid at δ 6.28 ppm were quantified. The reliability of the quantification method had been implemented successfully in validated experiments including specificity and selectivity, linearity, recovery, precision concentration rang, limit of detection (LOD), limit of quantification (LOQ), stability and robustness. Conclusion: The method was found to be liner (R2 = 0.9991) from 8.62 to 20.14 mg/0.6 mL DMSO-d6 in the drug concentration range. The maximum relative standard deviation (RSD) of recovery and precision were tested to be 0.59% and 0.65%, respectively. The LOD and LOQ were determined to be 0.02, 0.07 mg/mL, respectively. The RSD of stability was 0.05%. The robustness was demonstrated by changing four different parameters with the maximum difference less than 0.9%. In addition, the result of qNMR showed in good agreement with the HPLC and UV methods. Based on the experiments, the developed method was successfully applied to the determination of SSZ in commercial tablet.

DEVELOPMENT AND VALIDATION OF RAPID AND SIMPLE BIOANALYTICAL METHOD FOR DOCETAXEL WITH ONE STEP PROTEIN PRECIPITATION

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 23-32
Author(s):  
P. C. Mehendale ◽  
R. B Athawale ◽  
K. K. Singh ◽  
Keyword(s):  
Extraction Efficiency ◽  
Regression Coefficient ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Isocratic Elution ◽  
Limit Of Quantification ◽  
Extraction Solvent ◽  
One Step ◽  
Development And Validation

A rapid and simple bio-analytical method with one step protein precipitation and extraction using acetonitrile as extraction solvent was developed for docetaxel. The extraction efficiency was 87.81% with satisfactory separation of docetaxel and IS peaks by isocratic elution with C18 column (25 cm X 4.5 mm, 0.5μm), acetonitrile and water (53:47 % V/V) as a mobile phase at ambient temperature and flow rate of 1mL/min. Paclitaxel solution in acetonitrile (10 mcg/ mL) was used as internal standard. The calibration curve was linear over the concentration range 50 – 5000 ng/mL, regression coefficient R2= 0.99936 and slope 0.00034. The limit of quantification and limit of detection were found to be 33 ng/ mL and 100 ng/mL, respectively. Coefficient of variation for within day and between the days was in the range of 10.9 to 14.9 and 12.5 to 15.05, respectively. Accuracy of the method indicated % recovery of 97.92 – 104.24%. Thus, a precise, accurate and robust method was developed and validated as per FDA guidelines.

scholarly journals Development and Validation of an HPLC Method for the Analysis of Chlorpropham and 3-Chloroaniline in Potato Extracts

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Nidhal M. Sher Mohammed ◽  
T. H. Flowers ◽  
H. J. Duncan
Keyword(s):  
Limit Of Detection ◽  
Internal Standard ◽  
Potato Industry ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Repeated Injection ◽  
Good Separation ◽  
Limit Of Quantification ◽  
Development And Validation ◽  
Good Agreement

Chlorpropham (CIPC) is the main sprout inhibitor used by potato industry. There is concern about the residues of CIPC and its degradation product 3-chloroaniline, 3-CA; hence, analytical methods are required to analyse their residues in potato samples. An HPLC-UV method was developed and validated for the separation and quantification of these compounds using propham (IPC) as an internal standard. The chromatographic conditions required to achieve good separation were 60% mobile phase of methanol, 15-minute run time at a flow rate of 1.5 mL/min, and a detection wavelength of 210 nm using Phenomenex (ODS-2 250 mm × 4.60 mm 5 µm Sphereclone) column at an ambient temperature. The method was validated for precision, linearity, the limit of detection (LOD) and the limit of quantification (LOQ), producing high precision through RSD ≤ 0.03%, and acceptable criteria of the coefficient of determination (R2) of the calibration curves (0.990). LOD values of CIPC and 3-CA were approximately 0.01 µg/mL whereas the LOQ values were approximately 0.04 µg/mL using repeated injection approach. The proposed HPLC method was compared with the standard GC method of the CIPC residues extracted showing good agreement R2=0.99. Despite using the same extract, the recovery results for the proposed HPLC method were 13% higher than GC analysis.

scholarly journals Development and validation of a GC–MS method for the simultaneous determination of acetochlor, fluorochloridone, and pendimethalin in a herbicide emulsifiable concentrate formulation

2020 ◽  
Vol 32 (4) ◽  
pp. 238-241 ◽  
Author(s):  
Dandan Wang ◽  
Shengde Wu
Keyword(s):  
Internal Standard ◽  
Ternary Mixtures ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Limit Of Quantification ◽  
Emulsifiable Concentrate ◽  
Relative Standard ◽  
Replicate Measurements ◽  
Development And Validation

This paper describes a rapid method to simultaneously determine acetochlor, fluorochloridone and pendimethalin present in a herbicide emulsifiable concentrate (EC) formulation using gas chromatography–mass spectrometry (GC–MS). Selected ion monitoring mode was performed to increase the sensitivity, with dibutyl phthalate as an internal standard. The method was validated with respect to linearity, accuracy, precision, and stability. Chromatographic separation was carried out on a TG-5 MS column (30 m × 0.25 mm × 0.25 μm) with helium as the carrier gas at a flow rate of 1.0 mL/min. Calibration curves were linear over 2.0–20.0 μg/mL for each analyte, and the limit of quantification was below 20 ng/mL. Good performance in terms of recovery ranging from 94.5% to 102.5% at 3 concentration levels proved excellent accuracy. The intra- and inter-day relative standard deviations for 6 replicate measurements were always less than 5%. The developed method is simple and efficient for the routine determination of the ternary mixtures in a compound herbicide EC formulation product.

scholarly journals DEVELOPMENT AND VALIDATION OF CARBAMAZEPINE PLASMA CONCENTRATIONS MEASUREMENT AND ITS APPLICATION ON EPILEPSY PATIENTS

2017 ◽  
Vol 9 (9) ◽  
pp. 87 ◽  
Author(s):  
Astri Budikayanti ◽  
Chiswyta Chaliana ◽  
Melva Louisa ◽  
Rianto Setiabudy
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Plasma Concentrations ◽  
Internal Standard ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Development And Validation

Objective: To develop and validate high-performance liquid chromatography with photodiode array (HPLC-PDA) detector as a method for measuring carbamazepine plasma concentrations in epilepsy patients treated with monotherapy or polytherapy.Methods: Carbamazepine was extracted from epilepsy patients’ plasma through liquid-liquid extraction, using protein precipitation with chloroform. Analysis was performed using HPLC with Inertsil DS-4 C18 (4.6x150 mm), 5 μm particle size column. The optimal condition for separation was established in a mobile phase consisting of acetonitrile: water (50:50) at a flow rate of 1.0 ml/min, detected by PDA detector at 220 nm. Propylparaben was used as the internal standard. The retention time was 3.5 min.Results: Linearity was obtained over a concentration range of 0.5-16 μg/ml with r = 0.999. The method showed good intra-and inter-day precision and accuracy of more than 90% difference (% diff) and 95% relative standard deviation (RSD). Lower limit of quantification (LOQ) was 0.5 μg/ml and lower limit of detection (LOD) was 0.2 μg/ml with 100% accuracy and more than 90% precision. Recovery test was nearly 100%. Stability of carbamazepine plasma concentration in 3 epilepsy patients was measured on the first and third month of treatment, ranging between 83.5 to 98.7%. When used to compare carbamazepine as a monotherapy versus polytherapy, the method showed good selectivity.Conclusion: The present HPLC method was valid for measuring carbamazepine plasma concentrations in epilepsy patients treated with monotherapy or polytherapy. This method meets the standard in the EMEA guideline in terms of linearity, precision, and accuracy, also selectivity in epilepsy patients treated with polytherapy.

scholarly journals SaQuant: a real-time PCR assay for quantitative assessment of Staphylococcus aureus

2021 ◽  
Vol 21 (1) ◽  
Author(s):  
Colin Wood ◽  
Jason Sahl ◽  
Sara Maltinsky ◽  
Briana Coyne ◽  
Benjamin Russakoff ◽  
...  
Keyword(s):  
Staphylococcus Aureus ◽  
Sensitivity And Specificity ◽  
Pathogen Detection ◽  
Limit Of Detection ◽  
Future Research ◽  
Limit Of Quantification ◽  
Pathogen Prevalence ◽  
Single Well ◽  
Effective Public Health ◽  
Detection And Quantification

Abstract Background Molecular assays are important tools for pathogen detection but need to be periodically re-evaluated with the discovery of additional genetic diversity that may cause assays to exclude target taxa or include non-target taxa. A single well-developed assay can find broad application across research, clinical, and industrial settings. Pathogen prevalence within a population is estimated using such assays and accurate results are critical for formulating effective public health policies and guiding future research. A variety of assays for the detection of Staphylococcus aureus are currently available. The utility of commercial assays for research is limited, given proprietary signatures and lack of transparent validation. Results In silico testing of existing peer-reviewed assays show that most suffer from a lack of sensitivity and specificity. We found no assays that were specifically designed and validated for quantitative use. Here we present a qPCR assay, SaQuant, for the detection and quantification of S. aureus as might be collected on sampling swabs. Sensitivity and specificity of the assay was 95.6 and 99.9 %, respectively, with a limit of detection of between 3 and 5 genome equivalents and a limit of quantification of 8.27 genome equivalents. The presence of DNA from non-target species likely to be found in a swab sample, did not impact qualitative or quantitative abilities of the assay. Conclusions This assay has the potential to serve as a valuable tool for the accurate detection and quantification of S. aureus collected from human body sites in order to better understand the dynamics of prevalence and transmission in community settings.

scholarly journals Quantification of plasma remdesivir and its metabolite GS-441524 using liquid chromatography coupled to tandem mass spectrometry. Application to a Covid-19 treated patient

2020 ◽  
Vol 58 (9) ◽  
pp. 1461-1468 ◽  
Author(s):  
Jean-Claude Alvarez ◽  
Pierre Moine ◽  
Isabelle Etting ◽  
Djillali Annane ◽  
Islam Amine Larabi
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Half Life ◽  
Limit Of Detection ◽  
Treated Patient ◽  
Internal Standard ◽  
Therapeutic Drug ◽  
Active Metabolites ◽  
Limit Of Quantification ◽  
Positive Mode

AbstractObjectivesA method based on liquid chromatography coupled to triple quadrupole mass spectrometry detection using 50 µL of plasma was developed and fully validated for quantification of remdesivir and its active metabolites GS-441524.MethodsA simple protein precipitation was carried out using 75 µL of methanol containing the internal standard (IS) remdesivir-13C6 and 5 µL ZnSO4 1 M. After separation on Kinetex® 2.6 µm Polar C18 100A LC column (100 × 2.1 mm i.d.), both compounds were detected by a mass spectrometer with electrospray ionization in positive mode. The ion transitions used were m/z 603.3 → m/z 200.0 and m/z 229.0 for remdesivir, m/z 292.2 → m/z 173.1 and m/z 147.1 for GS-441524 and m/z 609.3 → m/z 206.0 for remdesivir-13C6.ResultsCalibration curves were linear in the 1–5000 μg/L range for remdesivir and 5–2500 for GS-441524, with limit of detection set at 0.5 and 2 μg/L and limit of quantification at 1 and 5 μg/L, respectively. Precisions evaluated at 2.5, 400 and 4000 μg/L for remdesivir and 12.5, 125, 2000 μg/L for GS-441524 were lower than 14.7% and accuracy was in the [89.6–110.2%] range. A slight matrix effect was observed, compensated by IS. Higher stability of remdesivir and metabolite was observed on NaF-plasma. After 200 mg IV single administration, remdesivir concentration decrease rapidly with a half-life less than 1 h while GS-441524 appeared rapidly and decreased slowly until H24 with a half-life around 12 h.ConclusionsThis method would be useful for therapeutic drug monitoring of these compounds in Covid-19 pandemic.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

Method Development and Validation of Spectrophotometric Methods for The Estimation of Rizatriptan Benzoate in Pure and Pharmaceutical Dosage Form

2021 ◽  
pp. 6003-6006
Author(s):  
Pushpa Latha E. ◽  
Sailaja B.
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Analytical UV derivative spectrophotometric method was developed and validated to quantify Rizatriptan Benzoate in pure drug and tablet dosage form. Based on the spectrophotometric characteristics of Rizatriptan Benzoate, a signal of zero (225nm), first (216nm), second (237nm), third (233nm), fourth (231nm) order derivative spectra were found to be adequate for quantification. The methods obeyed Beer's law in the concentration range of (0.1-360µg/ml) with square correlation coefficient (r2) of 0.999. The mean percentage recovery was found to be 100.01 ± 0.075. As per ICH guidelines the results of the analysis were validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification, and were found to be satisfactory.

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