Determination of residual phenylhydrazines in drug substances by high-performance liquid chromatography with pre-column derivatization

2019 ◽  
Vol 11 (48) ◽  
pp. 6146-6152
Author(s):  
Jiaxin Li ◽  
Eyoro Noah Nadine Joelle ◽  
Qian Yang ◽  
Feng Zheng ◽  
Wenyuan Liu ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Drug Substances ◽  
Genotoxic Impurities

A selective, sensitive and general HPLC method with pre-column derivatization was developed for the determination of residual phenylhydrazines (known as genotoxic impurities) in drug substances.

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

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.

Development of reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of selected antihypertensive active flavonoids (rutin, myricetin, quercetin, and kaempferol) in medicinal plants found in Botswana

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Katso Binang ◽  
David T. Takuwa
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Medicinal Plants ◽  
High Performance ◽  
Zingiber Officinale ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Lippia Javanica

Abstract The aim of the study was to develop a rapid, efficient, and cheap chromatographic method for determining four selected antihypertensive active flavonoid compounds in medicinal plants in Botswana. The determination of rutin, quercetin, and kaempferol in selected medicinal plants was conducted in less than 6 min using the developed reverse phase-high performance liquid chromatography (RP-HPLC) method with a 2.7 µm Ascentis C18 express column (150 × 4.60 mm i.d) at 340, 360, and 368 nm detection wavelengths and mobile phase of methanol and 0.068% of formic acid solution in isocratic elution. Validation results showed good selectivity, linearity (r 2 > 0.99), high percentage recoveries (90.2–104.7%), and precision (% RSD < 2) for n = 3, confirming suitability of the method for determination of the investigated flavonoids in Zingiber officinale (ginger). Application of the developed RP-HPLC method was performed in selected medicinal plants (Lippia javanica ) (mosukujane), Myrothanmus flabellious (galalatshwene), and Elephantorrhiza elephantina (mositsana) used to manage hypertension by herbalists in Botswana. M. flabellious a very commonly used plant for managing hypertension was found to contain highest amounts of rutin and myricetin, whereas nothing was detected for E. elephantina.

Establishment of an HPLC Method for Determination of Coumarin-3-Carboxylic Acid Analogues in Rat Plasma and a Preliminary Study on Their Pharmacokinetics

2021 ◽  
Author(s):  
Yan Xiong ◽  
Yong-Hong Liu ◽  
Jian-Sha Li ◽  
Yu-Ying Zhang ◽  
Jing Zhang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Carboxylic Acid ◽  
High Performance ◽  
Rat Plasma ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmacokinetic Parameters ◽  
Preliminary Study

Abstract A simple high performance liquid chromatography (HPLC) method was developed and validated for the determination of coumarin-3-carboxylic acid analogues (C3AA) in rat plasma and a preliminary study on pharmacokinetics. Ferulic acid (FA) was used as the internal standard substance, and coumarin-3-carboxylic acid (C3A) was used as a substitute for quantitative C3AA. After protein precipitation with methanol, the satisfactory separation was achieved on an ODS2 column when the temperature was maintained at 30 ± 2°C. The correlation coefficient r in the C3A linear equation is equal to 0.9990. Pharmacokinetic parameters for t1/2, Tmax, Cmax, area under the curve (AUC)0-t, average residence time (MRT), apparent volume of distribution (V z/F) and clearance (Cl/F) were 1.89 ± 0.03 h, 0.39 ± 0.14 h, 1.81 ± 0.10 g· mL−1 ·h, 7.88 ± 0.24 g·mL−1·h, 3.23 ± 0.14 h, 0.43 ± 0.03 (mg·kg−1)·(g·mL−1)−1·h−1, respectively. The high performance liquid chromatography-photo diode array detector (HPLC-PDA) method established in this study can be used to separate and determine the content of C3AA in plasma of rats after 60% ethanol extraction by gavage. The plasma concentration-time curve and pharmacokinetic parameters reflect the absorption of C3AA in rat blood after oral administration to some extent.

Development of a Method for the Determination of Pyrimethamine Concentrations in Feeds by Ion-Pairing High-Performance Liquid Chromatography

2002 ◽  
Vol 65 (4) ◽  
pp. 688-691 ◽  
Author(s):  
P. S. GONG ◽  
S. L. JENG ◽  
Y. F. HSU ◽  
C. C. LIN ◽  
S. Y. LIN
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Ion Pairing ◽  
Reversed Phase ◽  
Hplc Method ◽  
Alumina Column ◽  
Tetramethylammonium Chloride ◽  
Array Detection

An ion-pairing reversed-phase high-performance liquid chromatography (HPLC) method with diode array detection at 280 nm was developed to determine pyrimethamine concentrations in feed for laying hens. Pyrimethamine was extracted with a mixture of 5% isobutanol and 95% benzene, and the extract was cleaned up on an alumina column. The drug was eluted from an Intersil ODS-3V column (250 by 4.6 mm) with a mixture of 25% acetonitrile and 75% water (vol/vol) containing 0.01 M tetramethylammonium chloride as an ion-pairing agent and adjusted with acetic acid to pH 3.5. The flow rate was 1.0 ml/min. Mean recovery of pyrimethamine from supplemented feeds at concentrations of 2, 4, and 5 μg/g of feed were 100.5, 103.5, and 100.8%, respectively. Precision within a day ranged from 4.3 to 7.0% for the three concentrations, and day-to-day precision was 5.3% for feed supplemented at a concentration of 4 μg/g. No chromatographic interference was detected from other 2,4-diaminopyrimidine compounds or other major drugs used in poultry.

Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations

2020 ◽  
Vol 103 (5) ◽  
pp. 1223-1229
Author(s):  
Michikazu Tanio ◽  
Toru Nakamura ◽  
Hideki Kusunoki ◽  
Kyohei Ideguchi ◽  
Kazuyuki Nakashima ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Human Immunoglobulin ◽  
Histamine Dihydrochloride ◽  
Relative Standard

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R &gt; 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

scholarly journals Simultaneous Determination of 6 Antiallergic Components in Asarum sieboldii Using High-Performance Liquid Chromatography

2020 ◽  
Vol 15 (10) ◽  
pp. 1934578X2096619
Author(s):  
Seol Jang ◽  
Sun Haeng Park ◽  
Ho Kyoung Kim
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Inhibitory Effect ◽  
Hplc Method ◽  
Inhibitory Effects ◽  
Traditional Herbal Medicine ◽  
Simultaneous Quantification ◽  
Antiallergic Effect

Owing to the side effects of current drugs for treating atopic dermatitis (AD), a chronic disease in the skin, traditional herbal medicine is receiving much attention as an alternative treatment. Asarum sieboldii has traditionally been used to treat colds, fevers, headaches, coughs, neuralgia, chronic bronchitis, asthma, and allergies. In this study, 6 compounds (echinacoside, vanillic acid, kakuol, methyl eugenol, sesamin, and asarinin) in A. sieboldii were analyzed simultaneously using high-performance liquid chromatography (HPLC), and the proposed analytical method was validated. In addition, the inhibitory effects of the A. sieboldii extract and the 6 analyzed compounds on the expression of chemokine were evaluated in HaCaT cells. The HPLC method showed high linearity, with a correlation coefficient of ≥0.9999. The limits of detection for the 6 compounds ranged from 0.00 to 0.02 µg/mL, and the limits of quantification ranged from 0.01 to 0.05 µg/mL. The intraday and interday precisions were 0.15%-1.90%; the accuracy was 97.36%-103.23%, and the recoveries of the 6 compounds were 97.45%-103.93%. The content of each compound in A. sieboldii, as determined using the corresponding calibration curve, was in the range of 0.380-12.062 mg/g. This optimized simultaneous quantification method will be suitable for improving the quality control of A. sieboldii. Moreover, the 6 compounds in A. sieboldii showed an inhibitory effect on the production of chemokines, which suggests that A. sieboldii has an antiallergic effect.

HPLC Method for Determination of Ergot Alkaloids and Some Derivatives in Human Plasma

1985 ◽  
Vol 4 (6) ◽  
pp. 601-607 ◽  
Author(s):  
M. Žorž ◽  
J. Culig ◽  
Z. Kopitar ◽  
D. Milivojevic ◽  
A. Marušič ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Ergot Alkaloids ◽  
Hplc Method ◽  
Fluorometric Detection

1 Ergot alkaloids and their dihydrogenated methanesulphonate (ms) salts were determined and measured in human plasma. 2 High-performance liquid chromatography (HPLC) with fluorometric detection was used for separation of ergot alkaloids in plasma. 3 Several ergot alkaloids and their derivatives, including lysergide (LSD), can be identified in cases of poisoning.

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