scholarly journals Quantitative Determination of Azithromycin in Human Plasma by Liquid Chromatography–Mass Spectrometry and its Application in Pharmackokinetic Study

2012 ◽  
Vol 11 (1) ◽  
pp. 55-63 ◽  
Author(s):  
Maizbha Uddin Ahmed ◽  
Mohammad Safiqul Islam ◽  
Tasmin Ara Sultana ◽  
AGM Mostofa ◽  
Muhammad Shahdaat Bin Sayeed ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Solid Phase ◽  
Internal Standard ◽  
Extraction Process ◽  
Serum Samples ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Linear Concentration Range ◽  
Linear Concentration

Azithromycin is an effective and well-known antimicrobial agent. In the present study, a simple, sensitive and specific LC/MS/MS method has been developed and validated for the quantification of Azithromycin in  human serum samples using Clarithromycin as internal standard. Azithromycin was extracted from biological matrix  by using solid phase extraction process. The chromatographic separation was performed on Luna C18 (3 ?, 2x150   mm) column with a mobile phase consisting of 35 mM ammonium acetate buffer (mobile phase-A) and acetonitrile  and methanol in ratio of 90:10 ( as mobile phase-B) at a flow rate of 0.25 mL/min. The method was validated over a  linear concentration range of 0.5?50.0 ng/mL and limit of quantification (LOQ) was 0.5 ng/mL with a coefficient of  correlation (r2) = 0.9998. The intra-day and inter-day precision expressed as relative standard deviation were 1.64% – 8.43% and 2.32% – 9.92%, respectively. The average recovery of azithromycin from serum was 98.11%. The method  was successfully applied to a pharmacokinetic study after oral administration of Azithromycin 200 mg/5 ml suspension in healthy Bangladeshi volunteers. DOI: http://dx.doi.org/10.3329/dujps.v11i1.12488 Dhaka Univ. J. Pharm. Sci. 11(1): 55-63, 2012 (June)

Determination of PCB Residues in Vegetables by GC-MS

2012 ◽  
Vol 487 ◽  
pp. 724-729 ◽  
Author(s):  
Tie Bing Liu ◽  
Hai Yun Tu ◽  
Li Ming Han ◽  
Qiu Ping Yuan ◽  
Greg Duns
Keyword(s):  
High Speed ◽  
Polychlorinated Biphenyl ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Qualitative And Quantitative ◽  
Relative Standard ◽  
Combination Of Methods ◽  
Linear Concentration Range ◽  
Linear Concentration

This paper examines a method for the simultaneous detection of 12 different dioxin-like polychlorinated biphenyl (PCB) residues in vegetables. A qualitative and quantitative determination of PCB residues in vegetables was undertaken by a combination of high-speed freezing centrifugation, solid phase extraction, purification, concentration, and GC- MS and GC-ECD. From this combination of methods, 12 different PCBs were detected in vegetables over a linear concentration range of 0.001 to 2 µ g/L (ppb), with detection limits ranging from 0.4ppb to 0.5 ppb, a linear correlation coefficient of 0.99, recoveries ranging from 96.25%-117.5%, and a relative standard deviation ≤ 21%(RSD) .

scholarly journals Validation and Optimization of a Simple RP-HPLC Method for the Determination of Paracetamol in Human Serum and its Application in a Pharmacokinetic Study with Healthy Bangladeshi Male Volunteers

2015 ◽  
Vol 13 (2) ◽  
pp. 125-131
Author(s):  
Anisa Alam Tanam ◽  
Mohammad Firoz Khan ◽  
Ridwan Bin Rashid ◽  
Md Zakir Sultan ◽  
Mohammad A Rashid
Keyword(s):  
Human Serum ◽  
Pharmacokinetic Study ◽  
Internal Standard ◽  
Immediate Release ◽  
Hplc Method ◽  
Serum Samples ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

Acetaminophen (paracetamol) is an analgesic and antipyretic agent with minimum anti-inflammatory properties. In the present study a simple, fast, accurate, precise and reproducible RP-HPLC method has been developed and validated for the quantification of paracetamol in human serum samples using theophylline as internal standard. Protein precipitation with perchloric acid was employed in the extraction of paracetamol and theophylline from biological matrix. The chromatographic separation was accomplished on Phenomenex C18 column with a mobile phase comprising of 0.05 mM sodium sulfate buffer (pH 2.2 ± 0.02 adjusted with phosphoric acid) and acetonitrile at a ratio of 93:7 at a flow rate of 1.0 ml/min. The chromatogram was monitored by UV detection at a wavelength of 254 nm. The method was validated over a linear concentration range of 2-100 ?g/ml and limit of quantification (LOQ) was 1.61 ?g/ml with a correlation coefficient (r2) 0.997. The intra-day and inter-day precision expressed as relative standard deviation were found to be 0.49 - 2.68% and 0.36 - 3.44%, respectively. The average recovery of paracetamol from serum ranged from 99.0 - 106.4%. The method was successfully applied to a pharmacokinetic study after oral administration of immediate release paracetamol tablet (1000 mg) in four healthy Bangladeshi volunteers. The mean Cmax was found to be 11.03 ± 3.21 ?g/ml, which occurred at Tmax of 0.88 ± 0.14 hr. The half life, AUC0-8 and AUC0-? values were found to be 3.09 ± 0.71 hr, 31.06 ± 6.57 hr-?g/ml and 37.92 ± 9.51 hr- ?g/ml, respectively. DOI: http://dx.doi.org/10.3329/dujps.v13i2.21889 Dhaka Univ. J. Pharm. Sci. 13(2): 125-131, 2014 (December)

scholarly journals Determination of Trace Zearalenone and Its Metabolites in Human Serum by a High-Throughput UPLC-MS/MS Analysis

2019 ◽  
Vol 9 (4) ◽  
pp. 741 ◽  
Author(s):  
Danlei Sun ◽  
Chenglong Li ◽  
Shuang Zhou ◽  
Yunfeng Zhao ◽  
Yun Gong ◽  
...  
Keyword(s):  
Human Serum ◽  
High Throughput ◽  
Solid Phase ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Enzyme Hydrolysis ◽  
Serum Samples ◽  
Relative Standard ◽  
Before And After

This paper described an improved method for high-throughput and sensitive determination of zearalenone and its five metabolites (zearalanone, α-zearalenol, β-zearalenol, α-zearalanol and β-zearalanol) in human serum. Serum samples were measured both before and after enzyme hydrolysis to assess the free and total amount of each compound by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) in multi reaction monitoring (MRM) mode following off-line 96-well μElution solid-phase extraction (SPE). All the analytes were completely separated on a C18 column within 6 min. It enabled multi-sample preparation at the same time eliminating tedious evaporation and reconstitution steps, allowing 96 (one plate) samples to be processed and analyzed within 24 h. Using an isotope labelled internal standard (13C-ZEN), high recoveries were achieved for all the compounds in the range 91.6%–119.5%, with intra-day and inter-day relative standard deviations (RSDs) of less than 8%. The limits of detection (LOD) and the limits of quantification (LOQ) were 0.02–0.06 ng mL−1 (0.6–2 fmol) and 0.1–0.2 ng mL−1 (3–6 fmol), respectively, demonstrating a notable enhancement in sensitivity compared to the existing methods. The validated method was applied to the analysis of paired urine and serum samples collected from 125 healthy individuals in Henan Province, locating in the middle area of China. ZEN metabolites in human serum were significantly lower than those in urine. Only one serum sample was positive for ZEN after enzyme digestion, whereas at least one of ZEN biomarkers was detected in 75.2% of the paired urine samples. Some comparison and discussion were also included in this paper.

scholarly journals AN IMPROVED LC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF TRANDOLAPRIL AND VERAPAMIL IN HUMAN PLASMA

2019 ◽  
pp. 91-95
Author(s):  
YATHA RAVI ◽  
B. RAJKAMAL
Keyword(s):  
Method Development ◽  
Solid Phase ◽  
Internal Standard ◽  
Biological Matrix ◽  
Method Development And Validation ◽  
Ionization Mode ◽  
Development And Validation ◽  
Linear Concentration Range ◽  
Linear Concentration

Objective: A simple, sensitive and rapid LC-MS/MS technique was developed for the quantitation of trandolapril (TDL) and verapamil (VPL) in a biological matrix and validated. Methods: Sample preparation processed by SPE (Solid Phase extraction) on phenomenex cartridge using Ledipasvir as an internal standard. Two drugs were eluted on waters symmetry-RP18 (5µ, 150 mm×4.0 mm) column with the mobile composition of 10 mmol ammonium formate and ACN(acetonitrile) in the ratio of 70:30 %V/V. Detection and quantitation were processed by electrospray ionization in positive ionization mode. Results: The quantification approach was validated in 5-1500 ng/ml linear concentration range for TDL and 1-2000 ng/ml for VPL. The intraday and inter-day precision and accuracy were found to be 0.58% to 5.69% and 93% to 104% for two drugs. The average recoveries for TDL and VPL were found to be 92.9% and 93.5% respectively. Conclusion: The developed work was validated and can be applicable to the routine analysis of TDL and VPL simultaneously in a biological matrix.

Development and Validation of a New Method for the Determination of Anti-hepatitis C Agent Simeprevir in Human Plasma using HPLC with Fluorescence Detection

2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil
Keyword(s):  
Hepatitis C ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Assay Method ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Relative Standard

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

scholarly journals Determination of Fleroxacin in Pure and Tablet Forms by Liquid Chromatography and Derivative UV-Spectrophotometry

2003 ◽  
Vol 86 (2) ◽  
pp. 229-235 ◽  
Author(s):  
Dorota Kowalczuk ◽  
Hanna Hopkała
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Spectrophotometric Assay ◽  
Uv Spectrophotometry ◽  
Aminobenzoic Acid ◽  
Tetrabutylammonium Hydroxide ◽  
Relative Standard ◽  
Liquid Chromatographic ◽  
Derivative Uv Spectrophotometry

Abstract Derivative UV-spectrophotometric and liquid chromatographic (LC) methods for fleroxacin determination were validated. In the spectrophotometric assay, first-, second-, third-, and fourth-order measurements were applied with the use of peak–zero and peak–peak techniques. The linear correlation between amplitude of the peak and concentration of the examined drug ranged from 2.0 to 12.0 μg/mL. An isocratic LC analysis was performed on a Purospher ODS column with an acidic mobile phase containing tetrabutylammonium hydroxide. Measurements were made at a wavelength of 285 nm with 4-aminobenzoic acid (PABA) as internal standard. The calibration curve was linear (r = 0.9999) in the studied range of concentration (1.0–10.0 μg/mL). The accuracy (mean recovery, about 100%), precision (relative standard deviation &lt;1%), selectivity, and sensitivity of the elaborated methods were satisfactory.

scholarly journals Validated TLC-densitometry method for determination of cetirizine dihydrochloride in tablet dosage form

2013 ◽  
Vol 3 (1) ◽  
pp. 208-210
Author(s):  
Nia Kristiningrum ◽  
Ellsy Novita Martyanti
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Journal ◽  
Limit Of Quantification ◽  
Quality Control Testing ◽  
Relative Standard ◽  
Tablet Formulations ◽  
Tablet Dosage ◽  
Chloroform Methanol

A rapid, reproducible and accurate TLC method was developed for the determination of Cetirizine Dihydrochloride in tablet. The analytes were dissolved with ethanol 70% and chromatographed on silica Gel GF 254 TLC plate using chloroform : methanol : ethyl acetate in the ratio of 2 : 7 : 3 (v/v) as mobile phase. Quantitative analysis was done through densitometric measurement at wavelength 234 nm. Method was found linear over the concentration range of 400 – 1600 ng/spot with the correlation coefficient of 0.996. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 75.54 and 226.64 ng/spot. The relative standard deviation of this method was 0.86% whereas the means of the recovery data was 100.54 ± 0.11%. The proposed method has been applied to the determination of Cetirizine Dihydrochloride in commercial tablet formulations and the result were 96.97 ± 0.86 % for brand A and 100.57 ± 1.17 % for brand B. The developed method was successfully used for the assay of Cetirizine Dihydrochloride. This method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v3i1.17294 International Current Pharmaceutical Journal, December 2013, 3(1): 208-210

scholarly journals Rapid MSPD-LC–MS/MS Procedure for Determination of Pesticides in Potato Tubers

2020 ◽  
Vol 58 (9) ◽  
pp. 831-843
Author(s):  
Magdalena Danek ◽  
Marcin Sajdak ◽  
Joanna Płonka ◽  
Hanna Barchańska
Keyword(s):  
Analytical Procedure ◽  
Solid Phase ◽  
Potato Tubers ◽  
Limit Of Quantification ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Validation Parameters ◽  
Dispersion Technique

Abstract The program of potato protection recommended by the producers of agrochemicals requires application: thiamethoxam, lambda-cyhalothrin, deltamethrin, rimsulfuron and metalaxyl. Therefore, there is a risk that these pesticides are present in tubers, thus posing a toxicological risk to the consumer. In this respect, it is necessary to monitor the presence of these compounds in edible plants. Therefore, the aim of this paper was to develop a novel, simple and robust analytical procedure for simultaneous determination of above-mentioned pesticides in potato tubers. To develop an analytical procedure that fulfills SANTE demands, quick, easy, cheap, effective, rugged and safe method and matrix solid phase dispersion technique were investigated. The final determination was conducted by liquid chromatography with tandem mass spectrometry. The obtained experimental data were analyzed by analysis of variance. For the extraction of analytes, matrix solid phase dispersion with octadecyl sorbent and methanol as eluent was chosen, since it provides the validation parameters according to SANTE requirements (recovery: 77–111%, relative standard deviation: 1–10%, limit of quantification: 0.9–5.0 μg/kg). This innovative analytical procedure is a practical analytical tool, which was successfully proven by applying it for target pesticides determination in potato tuber samples of different varieties randomly chosen at local markets.

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