scholarly journals Internal Standard an Important Analyte Use in Drug Analysis by Liquid Chromatography Mass Spectrometry- An Article

2022 ◽  
Vol 02 (01) ◽  
Author(s):  
Pallab Mandal ◽  
Keyword(s):  
Internal Standard ◽  
Selection Procedure ◽  
Drug Analysis ◽  
Response Factor ◽  
Liquid Chromatography Mass Spectrometry ◽  
Analyte Concentration ◽  
Calibration Standard ◽  
Constant Concentration ◽  
Standard Curve ◽  
Clear Idea

Internal standard is an external compound which is mixed with targeted analytical solution and matrix as a constant concentration and use for preparing calibration standard curve by using ratio of analyte area and internal standard area with analyte concentration and internal standard concentration. This calibration curve used for quantification of unknown concentration of anlayte of interest. This article provide necessary information about internal standard like its selection procedure, characterization, types and response factor , to all analyst who are connected with drug analysis. This article is more important and I think first article which focuses a clear idea about internal standard use in drug analysis.

Method Development and Validation For Determining Stability of Omadacycline In Biological Matrices By Liquid Chromatography–Mass Spectrometry

2019 ◽  
Vol 10 (04) ◽  
pp. 640-645
Author(s):  
Satya Prasad B ◽  
Jaya Kumari S
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Precipitation Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Mobile Phase Composition ◽  
Column Temperature ◽  
Standard Curve ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Source Flow

The validated protein precipitation method was applied for the estimation of Omadacycline (OM) in human plasma with Omadacycline-D9 (OMD9) as an internal standard (ISTD) by using HPLC-ESI-MS/MS. Zorbax Eclipse Plus C18, 2.1 x 50 mm, 3.5 μm, was selected as the analytical column. The column temperature was set at 45°C. Mobile phase composition was 0.1% formic acid: methanol (80:20 v/v). Source flow rate of 300 μL/min without a split. An injection volume of 10 μL. Omadacycline and Omadacycline-D9 mesylate were eluted at 1.2 ± 0.2 min, with a total run time of 3.0 min for each sample. The mass transitions of Omadacycline and Omadacycline-D9 obtained were m/z 557.6 ® 456.6 and 566.7 ® 456.6, respectively. The standard curve shows a correlation coefficient (r2) greater than 0.9983 with a range of 5.00 to 12000.00 pg/ml using the linear regression model.

Development and Validation of a Liquid Chromatography/Mass Spectrometry Method for the Simultaneous Quantitation of Rosuvastatin and Ezetimibe in Human Plasma

2013 ◽  
Vol 96 (2) ◽  
pp. 307-312 ◽  
Author(s):  
Susheel John Varghese ◽  
Ravi Thengungal Kochupappy
Keyword(s):  
Human Plasma ◽  
Internal Standard ◽  
Liquid Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Spectrometry Method ◽  
Esi Ms ◽  
Standard Curve ◽  
Liquid Liquid Extraction ◽  
Development And Validation

Abstract A simple, rapid, and sensitive LC/electrospray ionization (ESI)-MS method was developed and validated for the simultaneous determination of rosuvastatin (ROS) and ezetimibe (EZE) in human plasma. Following liquid–liquid extraction, the analytes and an internal standard, atorvastatin (ATO), were separated using an isocratic mobile phase comprising 0.1% (v/v) formic acid–methanol (20 + 80, v/v) on an RP-C18 column. Detection was performed on a mass spectrometer by selected ion monitoring using their respective [M-H]– ions, m/z 480 for ROS, m/z 408 for EZE, and m/z 557 for ATO. For both analytes, the method was linear in the range of 0.1 to 10 ng/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 4 min made it possible to determine many plasma samples/day. The validated LC/ESI-MS method can be used to study pharmacokinetics, bioavailability, and bioequivalence of combined dosage forms of ROS and EZE.

Metabolic Analysis of Triptolide Microspheres in Human, Dog, Rabbit and Rat Liver Microsomes with UPLC-MS/MS Method

2020 ◽  
Vol 17 ◽  
Author(s):  
LiJuan Wang ◽  
Yan Liu ◽  
Rui Li ◽  
DongXian He
Keyword(s):  
Rat Liver ◽  
Liver Microsomes ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Liver Microsomes ◽  
Good Precision ◽  
Kinetics Parameters ◽  
Measure Concentration ◽  
Standard Curve ◽  
Variation Of Parameters

Objectives: Triptolide (TPL) has been shown to have a good clinical effect on rheumatoid arthritis (RA). We designed TPL microspheres (TPL-MS) and investigated its metabolic behavior in human, dog, rabbit and rat liver microsomes (HLM, DLM, RLM and SDRLM) with UPLC-MS/MS method. Methods: First, a UPLC-MS/MS method was established to measure concentration of TPL in samples. The sample was separated on a C18 column (2.1×100 mm, 1.8μm) and eluted with a gradient elution. The precursor ion/product ion were m/z 378.1/361.0 for TPL and 260.0/116.2 for the internal standard. Then T1/2, Vmax and CLint were calculated from the above data. Finally, the metabolites of TPL-MS were identified by high-resolution UPLC-MS/MS. The sample was separated on a C18 column (2.1×100 mm, 2.2 μm) and eluted with isocratic elution. Mass spectrometric detection was carried out on a thermo Q-exactive mass spectrometer with HESI. The scanning range of precursor ions was from m/z 50 to m/z 750. Result and Discussion: Through several indicators including standard curve, precision, accuracy, stability, matrix effect and recovery rate, the enzymatic kinetics parameters including T1/2, Vmax and CLint were completed. Several metabolites of TPL-MS were identified. Conclusion: UPLC-MS/MS method is an accurate and sensitive method for determination of TPL in liver microsome samples with good precision, accuracy and stability. The variation of parameters indicated that the microspheres can delay the elimination of TPL in liver microsomes. The metabolism of TPL-MS varied among species, but no new metabolites appeared.

scholarly journals Investigations on the Key Odorants Contributing to the Aroma of Children Soy Sauce by Molecular Sensory Science Approaches

Foods ◽  
2021 ◽  
Vol 10 (7) ◽  
pp. 1492
Author(s):  
Jia Huang ◽  
Haitao Chen ◽  
Zhiming Zhang ◽  
Yuping Liu ◽  
Binshan Liu ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Solid Phase ◽  
Internal Standard ◽  
Retention Indices ◽  
Soy Sauce ◽  
Gas Chromatography Mass Spectrometry ◽  
Volatile Components ◽  
Active Compounds ◽  
Standard Curve ◽  
Key Odorants

To investigate the key odor-active compounds in children’s soy sauce (CSS), volatile components were extracted by means of solvent extraction coupled with solvent-assisted flavor evaporation (SE-SAFE) and solid-phase microextraction (SPME). Using gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS), we identified a total of 55 odor-active compounds in six CSSs by comparing the odor characteristics, MS data, and retention indices with those of authentic compounds. Applying aroma extract dilution analysis (AEDA), we measured flavor dilution (FD) factors in SE-SAFE isolates, ranging from 1 to 4096, and in SPME isolates, ranging from 1 to 800. Twenty-eight odorants with higher FD factors and GC-MS responses were quantitated using the internal standard curve method. According to their quantitated results and thresholds in water, their odor activity values (OAVs) were calculated. On the basis of the OAV results, 27 odorants with OAVs ≥ 1 were determined as key odorants in six CSSs. These had previously been reported as key odorants in general soy sauce (GSS), so it was concluded that the key odorants in CSS are the same as those in GSS.

scholarly journals NEW METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF FEBUXOSTAT IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY

2016 ◽  
Vol 8 (9) ◽  
pp. 61 ◽  
Author(s):  
Narottam Pal ◽  
Avanapu Srinivasa Rao ◽  
Pigilli Ravikumar
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
New Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

<p><strong>Objective</strong>:<strong> </strong>To develop a new method and validate the same for the determination of Febuxostat (FBS) in human plasma by liquid chromatography–mass spectrometry (LCMS).</p><p><strong>Methods</strong>:<strong> </strong>The present method utilized reversed-phase high-performance liquid chromatography with tandem mass spectroscopy. Febuxostat D9 (FBS D9) was used as internal standard (IS). The analyte and internal standard were separated from human plasma by using solid phase extraction method. Zorbax Eclipse XDB, C<sub>8</sub>, 100 mm x 4.6 mm, 3.5 µm column was used and HPLC grade acetonitrile, 5 millimolar (mM) ammonium format (80: 20, v/v) as mobile phase, detected by mass spectrometry operating in positive ion and multiple reaction monitoring modes.</p><p><strong>Results</strong>:<strong> </strong>The parent and production transitions for FBS and internal standard were at m/z 317.1→261.0 and 326.1→262.0 respectively. The method was validated for system suitability, specificity, carryover effect, linearity, precision, accuracy, matrix effect, sensitivity and stability. The linearity range was from 20.131 ng/ml to10015. 534 ng/ml with a correlation coefficient of 0.999. Precision results (%CV) across six quality control samples were within the limit. The percentage recovery of FBS and internal standard from matrix samples was found to be 76.57% and 75.03% respectively.</p><p><strong>Conclusion</strong>:<strong> </strong>Present study describes new LC-MS method for the quantification of FBS in a pharmaceutical formulation. According to validation results, it was found to be a simple, sensitive, accurate and precise method and also free from any kind of interference. Therefore the proposed analytical method can be used for routine analysis for the estimation of FBS in its formulation.</p>

Seasonal variation of abscisic acid in the dormant shoots of Douglas-fir

1979 ◽  
Vol 57 (5) ◽  
pp. 534-538 ◽  
Author(s):  
Joe E. Webber ◽  
Murray L. Laver ◽  
Joe B. Zaerr ◽  
Denis P. Lavender
Keyword(s):  
Abscisic Acid ◽  
Liquid Chromatography ◽  
Seasonal Variation ◽  
Internal Standard ◽  
Close Correlation ◽  
Douglas Fir ◽  
Gas Liquid Chromatography ◽  
Bud Burst ◽  
Liquid Chromatography Mass Spectrometry ◽  
Layer Chromatography

The occurrence of abscisic acid (ABA) in the dormant shoots of Douglas-fir (Pseudotsuga menziesii (Mirb.) Franco) was confirmed by bioassay, thin-layer chromatography, gas–liquid chromatography, and gas–liquid chromatography – mass spectrometry. Seasonal variation of ABA in the buds, leaves, and stems was then determined using 2-trans-ABA as an internal standard. Concentrations of ABA were highest in the autumn for buds (2.1 μg/g) and needles (0.79 μg/g) and highest in January for stems (0.34 μg/g). The lowest concentrations for all tissues were in February and March, before bud burst. Close correlation of levels of ABA with previously measured physiological evidence of growth and metabolic activity suggests a possible role in the dormancy cycle of Douglas-fir.

Determination of Volatile Organic Contaminants in Bulk Oils (Edible, Injectable, and Other Internal Medicinal) by Purge-and-Trap Gas Chromatography/Mass Spectrometry

1994 ◽  
Vol 77 (3) ◽  
pp. 647-654 ◽  
Author(s):  
Don W Thompson
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Vegetable Oils ◽  
Organic Contaminants ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Purge And Trap ◽  
Standard Curve ◽  
Volatile Organic ◽  
Volatile Organic Contaminants

Abstract Purge-and-trap gas chromatography/mass spectrometry is evaluated for the quantitation of part-per-billion levels of volatile organic contaminants in bulk vegetable oils. Results using 2 purge techniques (direct purging of the heated oil and purging after dispersing the oil on an aluminum oxide powder) and 2 quantitative methods (standard curve and deuterium-labeled internal standard addition) are reported. Twenty volatile compounds and 8 vegetable oils were investigated. Recovery data and estimated detection limits for each compound are reported for each purge technique. Generally acceptable recoveries (70-130% for more than 90% of the analyte spikes) and acceptable detection levels (approximately 4-10 ppb) were obtained for all compounds using either the external standard curve or the deuterium-isotope-labeled internal standard. The use of a dispersant (such as alumina) for sample purging resulted in poor recoveries of the highly volatile contaminants.

Analysis of Myo-inositol in Dry Beans by Gas Chromatography of Its Hexaacetate

1972 ◽  
Vol 55 (6) ◽  
pp. 1194-1198
Author(s):  
Richard M Seifert
Keyword(s):  
Mass Spectrometry ◽  
Internal Standard ◽  
Peak Height ◽  
Chromatographic Retention ◽  
Gas Liquid Chromatography ◽  
Standard Curve ◽  
Pinto Bean ◽  
White Bean ◽  
Pinto Beans ◽  
Hydrolysis Of

Abstract A method has been developed for the analysis of myo-inositol in California small white beans, pinto beans, and 2 pinto bean flake products by gas-liquid chromatography of myo-inositol hexaacetate. The identity of myoinositol hexaacetate from bean samples was confirmed by mass spectrometry and chromatographic retention time. A standard curve prepared by plotting peak height vs. μg myoinositol hexaacetate was linear over the range studied, 0.2 to 0.6 μg. Peak heights were measurable in all samples, although inositol hexaacetate was not completely separated in California small white bean samples. An internal standard, perseitol, was used to correct for losses in the procedure. Hydrolysis of phytin was negligible during sample preparation or analysis. Recoveries of 12 to 40 μg inositol from 40 mg samples of California small white beans averaged 113%. These beans contained an average of 71 ppm inositol compared to 215 ppm inositol in similarly prepared pinto beans.

scholarly journals Simultaneous Determination of Levocetirizine and Pseudoephedrine in Dog Plasma by Liquid Chromatography-Mass Spectrometry in the Presence of Dextrocetirizine

2012 ◽  
Vol 15 (4) ◽  
pp. 519 ◽  
Author(s):  
Jae Kuk Ryu ◽  
Sun Dong Yoo
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Oral Administration ◽  
Mobile Phase ◽  
Internal Standard ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chiral Column ◽  
Accuracy And Precision ◽  
Dog Plasma

Purpose. This study describes the development of a rapid and sensitive LC-ESI-MS assay for simultaneous enantioselective determination of levocetirizine and pseudoephedrine in dog plasma in the presence of dextrocetirizine. Methods. Separations were achieved on an Ultron ES-OVM chiral column using the mobile phase consisting of 10 mM aqueous NH4OAc (pH 6.6) and acetonitrile (9:1 v/v). Results. The retention times of pseudoephedrine, dextrocetirizine, levocetirizine and diazepam (internal standard) were 5.2, 8.3, 9.6 and 11.6 min, respectively, and the total run time was less than 15 min. The assay was validated to demonstrate the linearity, accuracy and precision, recovery and stability. The calibration curves were linear over the concentration range from 1 – 200 ng/mL for levocetirizine and from 5 – 1000 ng/mL for pseudoephedrine. Conclusions. The developed assay was successfully applied to a pharmacokinetic study after oral administration of the racemic cetirizine (0.5 mg/kg, or 0.25 mg/kg as levocetirizine) and pseudoephedrine (12 mg/kg) in the dog. This article is open to POST-PUBLICATION REVIEW. Registered readers (see “For Readers”) may comment by clicking on ABSTRACT on the issue’s contents page.

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