Validation of Analytical Methods for Tacrolimus Determination in Poly(ε-caprolactone) Nanocapsules and Identification of Drug Degradation Products

2021 ◽  
Vol 21 (12) ◽  
pp. 5920-5928
Author(s):  
Guilherme A. Camargo ◽  
Amanda M. Lyra ◽  
Fernanda M. Barboza ◽  
Barbara C. Fiorin ◽  
Flávio L. Beltrame ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Multiple Reaction Monitoring ◽  
Forced Degradation ◽  
Alkaline Stress ◽  
Drug Degradation ◽  
Relative Standard ◽  
Polymeric Nanocapsules ◽  
Alkaline Conditions

The aim of this paper was to use chromatographic tools for validating an analytical method for the tacrolimus (TAC) determination in polymeric nanocapsules and for identifying the drug degradation products after alkaline stress. A rapid Ultra-High-Performance Liquid Chromatography coupled with photo-diode array (UHPLC-PDA) method was successfully performed using the following chromatographic conditions: the Shimadzu Shim-pack XR-ODS III C18 column (100 mm×2.00 mm, 2.2 μm), the mobile phase consisting of methanol and acidified ultrapure water (89:11 v/v), the flow rate of 0.55 mL·min−1, and the ultraviolet (UV) detection at 235 nm. This method was validated as per International Council for Harmonisation (ICH) guidelines. In addition, a TAC forced degradation assay was carried out after alkaline stress and its degradation products were investigated using Liquid Chromatography coupled tandem mass spectroscopy (LC-MS/MS). The calibration curve was linear in the range of 100.0–300.0 μg·mL−1 (r >0.9999). Accuracy was confirmed by the TAC recovery of 96.55 to 98.19%. Precision (intraday and interday) were demonstrated by relative standard deviation lower than 0.89% and 3.25%, respectively. Selectivity and robustness were also proved. The method developed it was successfully applied to quantify TAC from polymeric nanocapsules, showing a high loading efficiency rate (>96.47%). The main drug degradation product observed in a multiple reaction monitoring (MRM) experiment was m/z 844, confirming the susceptibility of TAC under alkaline conditions; this finding was first time described.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

scholarly journals Dissipation Kinetics and the Pre-Harvest Residue Limits of Acetamiprid and Chlorantraniliprole in Kimchi Cabbage Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2019 ◽  
Vol 24 (14) ◽  
pp. 2616
Author(s):  
Jonghwa Lee ◽  
Byung Joon Kim ◽  
Eunhye Kim ◽  
Jeong-Han Kim
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Dissipation Kinetics ◽  
Relative Standard ◽  
Harvest Residue

The dissipation behaviors of acetamiprid and chlorantraniliprole in kimchi cabbages were studied under open-field conditions. A simple and rapid analytical method was developed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The multiple reaction monitoring (MRM) conditions of two pesticides were optimized to quantify and identify the pesticide residues. Sample preparation was performed by the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method. Average recovery rates at the different spiked levels (0.05 and 0.25 mg/kg) were in the range of 103.6–113.9% (acetamiprid) and 80.8–91.2% (chlorantraniliprole), and the relative standard deviations were ≤4.3% for all. The dissipation kinetics were assessed using first-order equations after spraying acetamiprid and chlorantraniliprole individually on kimchi cabbages. The biological half-lives in field 1 and 2 were 5.2 and 6.3 days (acetamiprid) and 10.0 and 15.2 days (chlorantraniliprole), respectively. Based on the dissipation equations, the pre-harvest residue limits (PHRLs) corresponding to each day before harvest were suggested as the guidelines to meet the MRL on harvest day. It was also predicted that the terminal residues observed after multiple sprayings (three and seven days) would be below the MRL when harvested, in compliance with the established pre-harvest intervals.

Determination of a Yellow Rice Toxin, Luteoskyrin, in Rice by Using Liquid Chromatography–Tandem Mass Spectrometry with Electrospray Ionization

2009 ◽  
Vol 72 (6) ◽  
pp. 1321-1326 ◽  
Author(s):  
KOHEI MIZUTANI ◽  
SUSUMU KUMAGAI ◽  
NAOKI MOCHIZUKI ◽  
YASUSHI KITAGAWA ◽  
YOSHIKO SUGITA-KONISHI
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Electrospray Ionization ◽  
High Performance ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Phase System ◽  
Ionization Mass ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard

Penicillium islandicum produces luteoskyrin (LUT), a yellow rice toxin that has been found frequently in rice. However, conventional analytical methods for determining LUT are limited, are complicated, and exhibit low sensitivity. In this study, an analytical method more sensitive and simple based on high-performance liquid chromatography combined with electrospray ionization mass spectrometry was developed. The cleanup procedure of the method was one step, using a solid-phase extraction cartridge. An isocratic mobile-phase system, consisting of acetonitrile–water–acetic acid (50:49:1 [vol/vol/vol]) at a flow rate of 0.2 ml/min, was utilized to obtain the best resolution. Our method showed good linearity (r = 0.9993, 0.5 to 50 ng/g) and high repeatability (relative standard deviation = 8.9 and 5.1% at levels of 0.5 and 10 ng/g, respectively) in the fortification test. The detection and quantification limits for the method in multiple-reaction monitoring mode were 0.1 and 0.3 ng/g, respectively. The average recovery of LUT in spiked rice at 0.5 and 10 ng/g was 80.7 and 85.2%, respectively. The method developed in this study should be applicable to survey LUT in rice, with high sensitivity, selectivity, and rapidity.

scholarly journals A NEW HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SEPARATION AND SIMULTANEOUS QUANTIFICATION OF EPTIFIBATIDE AND ITS IMPURITIES IN PHARMACEUTICAL INJECTION FORMULATION

2021 ◽  
pp. 165-172
Author(s):  
K. SRI GIRIJA ◽  
BIKSHAL BABU KASIMALA ◽  
VENKATESWARA RAO ANNA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Ultra Violet ◽  
Hplc Method ◽  
Chromatography Method ◽  
Standard Drug ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard

Objective: The objective of the present study is to develop a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for qualitative and quantitative determination of Eptifibatide and its impurities in bulk and pharmaceutical dosage forms. Methods: The chromatographic separation was carried on Phenomenex Luna C18 column (250 mm×4.6 mm; 5µ id) as stationary phase, methanol and phosphate buffer at pH 6.4 in the ratio of 65:45 (v/v) as mobile phase at flow rate of 1.0 ml/min, Ultra Violet (UV) detection was carried at the wavelength of 236 nm and the analysis was completed with a run time of 15 min. Results: In the developed conditions, the retention time of Eptifibatide and its impurities 1 and 2 were found to be 3.35, 4.93 and 8.18 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50%, 100% and 150% was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for Eptifibatide and both impurities studied and the % Relative standard deviation (RSD) in each spiked level was found to be less than 2. Stability tests were done through the exposure of the analyte solution to five different stress conditions i. e expose to 1N Hydrochloric acid (HCl), 1 N Sodium hydroxide (NaOH), 3% Hydrogen peroxide (H2O2), 80 °C temperature to UV radiation. In all the degradation conditions, standard drug Eptifibatide was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis, there is no other chromatographic detection of other impurities and formulation excipients. Conclusion: The developed method was found to be suitable for the quantification of Eptifibatide and can separate and analyse impurities 1 and 2.

scholarly journals BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ENTRECTINIB IN RAT PLASMA BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY

2020 ◽  
pp. 155-163
Author(s):  
PRAVALLIKA KE ◽  
PRAMEELA RANI A ◽  
RATNA KUMAR M
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Array Detector ◽  
Pharmaceutical Drugs ◽  
Relative Standard

Objective: The objective of the study was to develop and validate the bioanalytical liquid chromatography–mass spectrometry (LCMS/MS) method for the estimation of entrectinib in bulk and pharmaceutical drugs in rat plasma. Methods: Chromatographic separation of entrectinib with D4-entrectinib as internal standard (IS) was achieved using Waters Alliance high-performance liquid chromatography system, quaternary gradient pump of e2695, using Luna, 250×4.6 mm, 5 μm column and the mobile phase containing 0.1% formic acid and acetonitrile (ACN) within the ratio of 70:30% v/v. The flow was 1.0 ml/min; detection was carried out by absorption at 294 nm using a photodiode array detector at ambient temperature. Results: The peak of entrectinib was eluted at retention times of 5.225 min. The multiple reaction monitoring was 560.6/475.1 (m/z) for entrectinib and 580.6/496.3 (m/z) for IS entrectinib (D4). The linearity range was 1–20 ng/ml with a regression coefficient of 0.999. % relative standard deviation of peak areas of all measurements always <2.0. Conclusion: The method was successfully validated and it had been found to be within limits for accuracy, precision, and linearity and it is stable under analytical conditions used.

scholarly journals A Rapid Determination and Quantification of Three Biologically Active Polyisoprenylated Benzophenones using Liquid Chromatography-Tandem Mass Spectrometry (MRM) Method in Five Garcinia species from Cameroon

2017 ◽  
Vol 12 (12) ◽  
pp. 1934578X1701201
Author(s):  
Bernadette Messi Biloa ◽  
Raimana Ho ◽  
Guillaume Marti ◽  
Alain Meli Lannang ◽  
Jean-Luc Wolfender ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Rapid Determination ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Biologically Active ◽  
Ionization Mass ◽  
Relative Standard

Following investigation of Garcinia genus, a sensitive, rapid and simple reversed-phase high performance liquid chromatography-electrospray ionization mass spectrometry method has been developed for the identification and quantification of three polyisoprenylated benzophenones, garcinol (1), isogarcinol (2) and 7- epi-clusianone (3), in the extracts of five Garcinia species from Cameroon. The separation of those compounds was achieved on a RP-18 column using a solvent system consisting of a mixture of acetonitrile-water-formic acid as a mobile phase in a gradient elution mode. The identification of the three compounds was determined on a triple quadripole mass spectrometer with ESI interface operating in the negative mode. A multiple reaction monitoring (MRM) method was developed for the quantification of these polyisoprenylated benzophenones in the extracts of the Garcinia species. The method was validated through intra- and inter-day precision, with the relative standard deviation (RSD) less than 6%, limits of detection (LOD) and limits of quantification (LOQ) <1 ng. Overall recoveries ranged from 94% to 104%, with RSDs ranging from 0.8% to 4.5%. The results indicated that the fruits of G. preussii and the roots of G. brevipedicellata are good source of garcinol (1) and isogarcinol (2) respectively.

scholarly journals Validated Column High-Performance Liquid Chromatographic Method for Determination of Aspirin and Clopidogrel in Combined Tablets in the Presence of Degradation Products Formed Under ICHRecommended Stress Conditions

2009 ◽  
Vol 92 (1) ◽  
pp. 152-157 ◽  
Author(s):  
Pankaj K Kachhadia ◽  
Ashish S Doshi ◽  
Hitendra S Joshi
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Parent Compound ◽  
High Performance Liquid Chromatographic ◽  
Stress Conditions ◽  
Assay Method ◽  
Forced Degradation ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract The development and validation of a column high-performance liquid chromatographic assay method for the determination of aspirin and clopidogrel in tablet formulation are described. The combination formulation was subjected to International Conference on Harmonization-recommended stress conditions. Separation of the drugs from the degradation products formed under stress conditions was achieved on an octasilyl (C8) column using 0.3 orthophosphoric acidacetonitrile (65 + 35, v/v) mobile phase. The method was validated for specificity, linearity, limits of detection and quantification, precision, accuracy, and robustness. The method was found to be specific against placebo interference and during the forced degradation. The response was linear in the concentration range of 30.0120.0 g/mL for aspirin and 15.060.0 g/mL for clopidogrel, with a correlation coefficient of 0.9999 for both. The relative standard deviation values for intra- and interday precision were &lt;2.0. The accuracy was between 99.12 and 99.83 for aspirin and 98.20 and 100.35 for clopidogrel. Stress testing showed degradation products that were well-separated from the parent compound, confirming the stability-indicating capacity of the method.

scholarly journals Rapid Determination of Chloramphenicol in Tilapia by ultra-high performance liquid chromatography-mass spectrometry

2019 ◽  
Vol 78 ◽  
pp. 02005
Author(s):  
Shaodong Zeng ◽  
jianzhi Ye ◽  
Ling Lin ◽  
wuhai Chen ◽  
Chunliang Yang
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Rapid Determination ◽  
Water Solution ◽  
Multiple Reaction Monitoring ◽  
High Sensitivity ◽  
Relative Standard

A rapid method for the determination of residues of chloramphenicol in tilapia by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The samples were extracted with acetonitrile, and separated on a C18 column using methanol-water solution as mobile phase, and then detected under ESI- multiple reaction monitoring mode. The method showed a good linearity for the analysts over the range of 0.1-100μg/L. The detection limits were 0.10μg/kg. The recoveries ranged from 88.6% to 108% at spiked concentrations with the relative standard deviations lower than 5%. The results shows that this method has the advantages of easy to operate, fast to perform, with high sensitivity and accuracy, and it is suitable for detection of residues of chloramphenicol in tilapia.

scholarly journals Development and Validation of a New High-Performance Liquid Chromatography Method for the Determination of Gliclazide and Repaglinide in Pharmaceutical Formulations

2006 ◽  
Vol 89 (2) ◽  
pp. 319-325 ◽  
Author(s):  
Anna Berecka ◽  
Anna Gumieniczek ◽  
Hanna Hopkaa
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Pharmaceutical Formulations ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Total Recovery ◽  
Relative Standard ◽  
Liquid Chromatography Method

Abstract A new high-performance liquid chromatography method was developed and validated for the quantitation of gliclazide and repaglinide in pharmaceutical formulations. Determination was performed using a LiChroCART RP-18 column, a mobile phase containing acetonitrilephosphate buffer (pH 2.1; 60 + 40, v/v), and ultraviolet (UV) detection at 225 nm. Repaglinide was used as an internal standard for gliclazide determination and gliclazide for repaglinide assay. The method was validated with respect to linearity, precision, robustness, ruggedness, accuracy, and specificity. The calibration graphs ranged from 0.015 to 0.09 mg/mL for gliclazide and 0.06 to 0.36 mg/mL for repaglinide. Intra- and interday relative standard deviation values for the standard solutions were 0.70 and 1.01% for gliclazide and 0.78 and 0.93% for repaglinide, respectively. Total recoveries of gliclazide and repaglinide from the laboratory-prepared mixtures were 99.82 0.58 and 101.50 0.46% for gliclazide and repaglinide, respectively (mean standard deviation (SD)]. In forced degradation studies, the effect of acid, base, oxidation, UV light, and temperature on both drugs was also investigated. Finally, the method was applied for the quality control of commercial gliclazide and repaglinide tablets. Total recovery was 100.40 0.35 and 104.46 0.23% f SD). or gliclazide and repaglinide, respectively [mean SD).

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