scholarly journals Determination of the Contents of Antioxidants and Their Degradation Products in Sodium Chloride Injection for Blood Transfusion

2020 ◽  
Vol 2020 ◽  
pp. 1-12
Author(s):  
Bo Tao ◽  
Gang Wang ◽  
Zongning Yin ◽  
Xiaocong Pu ◽  
Yan Jiang ◽  
...  
Keyword(s):  
Sodium Chloride ◽  
Blood Transfusion ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Daily Intake ◽  
Gradient Elution ◽  
Hplc Method ◽  
Polymer Materials ◽  
Limit Of Quantification ◽  
Column Temperature

The infusion bag is mainly made up of polyolefin polymer. Antioxidants are usually added to these polymer materials in the production process to prevent the materials from aging and enhance the stability of the materials. Because of the potential harm of antioxidants to human body, it is necessary to limit the amount of antioxidants migrating to the pharmaceutical solutions. In the present study, we developed and validated the HPLC method for the simultaneous quantification of antioxidants and their degradation products migrating to sodium chloride solution for injection. A total of six antioxidants and six their degradation products were separated and simultaneously determined by using a Waters Symmetry RP18 column (250 × 4.6 mm, 5 μm) and gradient elution of methanol/acetonitrile/acetic acid-water (1 : 99, v/v) at a flow rate of 1.0 mL/min. The detective wavelength was set at 277 nm, and the column temperature was maintained at 35°C. The method was validated in terms of limit of detection (LOD, 0.011–0.151 μg/mL), limit of quantification (LOQ, 0.031–0.393 μg/mL), intraday precision (0.25%–3.17%), interday precision (0.47%–3.48%), linearity (0.1–46.8 μg/mL, r > 0.9994), stability (0.35%–3.29%), and accuracy (80.39%–104.31%). In the extraction experiment, antioxidants, BHT, 1010, 1330, 1076, and 168, and their degradation products, 1310 and DBP, were detected in the packaging materials. Only 1310 was detected in the migration experiment. The maximum daily dosage of sodium chloride for blood transfusion is three bags, and the content of 1310 in long-term testing samples is from 0 to 12 months ranging from 37.44 μg/3 bags to 48.71 μg/3 bags. The daily intake of 1310 did not exceed 48.71 μg, which was much lower than its permitted daily exposure (PDE, 300 μg/day). Therefore, the antioxidants and their degradation products migrating into the drug solution would not cause drug safety risks.

scholarly journals Development and Validation of New RP-HPLC Method for Simultaneous Determination of Methyl and Propyl Parabens with Levetiracetam in Pure Form and Pharmaceutical Formulation

2016 ◽  
Vol 2016 ◽  
pp. 1-5 ◽  
Author(s):  
Soad S. Abd El-Hay ◽  
Mostafa S. Mohram
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Limit Of Quantitation

A simple and robust high-performance liquid chromatography (HPLC) method is described for the assay for levetiracetam (LTC), methyl paraben (MHB), and propyl paraben (PHB) either in their pure form or in commercial Levepsy® syrup. The method is selective and stability indicating and all chromatographic conditions were studied to obtain adequate separation of LTC, MHB, and PHB from their degradation products and from excipients. The HPLC separation was carried out on a RP C18 Hypersil BDS analytical column (150 mm × 4.6 mm ID) using gradient elution system. The mobile phase flow rate was 1.5 mLmin−1 and the column temperature was kept at 40°C. Complete separation of the studied components was obtained within a cycle time of 8 min. LTC, MHB, and PHB were eluted at 1.56, 5.86, and 7.85 min, respectively. Detection was carried out at 240 nm using a dual wavelength detector. The method has been validated for linearity, accuracy, precision, specificity, limit of detection, limit of quantitation, robustness, and ruggedness. The proposed method was successfully applied for the determination of LTC in the presence of parabens in Levepsy syrup.

Rapid Determination of Amygdalin and its Novel Degradation Product in Plasma of Mice by SPE-HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 83-88
Author(s):  
Chen Xi Wang ◽  
Yu Ping Li ◽  
Jun Chang ◽  
Bin Zhou ◽  
Xiao Han ◽  
...  
Keyword(s):  
Formic Acid ◽  
Extracellular Enzymes ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Gradient Elution ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
High Antitumor Activity ◽  
Set Up

Amygdalin was catalytic degraded by extracellular enzymes mixture from Aspergillus niger and a novel product, phenyl-(3,4,5-trihydroxy-6-methyl-tetrahydro-pyran-2-yloxy)-acetonitrile (PTMT), with high antitumor activity was identified and purified. To measured the Pharmacokinetic of amygdalin and its products, a simple and rapid SPE-HPLC method was set up. The analysis was performed on an Agilent HPLC system with a C18 ODS column (250 × 4.6 mm i.d.) by gradient elution with 0.05% formic acid in water and 0.05% formic acid in acetonitrile as the gradient mixtures. The flow rate was 1ml/min, the detection wavelength was 215 nm and the column temperature was kept at 25°C. The HPLC assay was carried out within 9 min. The retention times of amygdalin, mandelonitrile, prunasin, PTMT andbenzaldehyde were 3.14, 5.93, 6.82, 7.35 and 8.33 min, respectively. The mean absolute recoveries of three analysts were over 98%. The limit of detection and limit of quantification for were 0.02 and 0.04 μg/ml for amygdalin and benzaldehyde, 0.03 and 0.05 μg/ml for mandelonitrile, and 0.03 and 0.04 μg/ml for prunasin and PTMT.

STABILITY INDICATING UPLC METHOD FOR ESTIMATION OF METFORMIN HYDROCHLORIDE AND NATEGLINIDE SIMULTANEOUSLY IN THE PRESENCE OF STRESS DEGRADATION PRODUCTS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (05) ◽  
pp. 56-64
Author(s):  
Rani A Prameela ◽  
S. Madhavi ◽  
Rao B. Tirumaleswara ◽  
Sudheer Reddy CH.
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Metformin Hydrochloride ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Column Temperature

A novel Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the simultaneous determination of antidiabetic drugs metformin hydrochloride and nateglinide. The method was developed using a Waters ACQUITY UPLC SB C18 (100 × 2.1 mm, 1.8 μm) column. The mobile phase consisting of 0.01 % potassium dihydrogen phosphate buffer (pH 5.8): acetonitrile (50: 50 V/V) was used throughout the analysis. The flow rate was 0.3 mL/min, the injection volume was 1.0 μL, column temperature was 30 0C, run time 3 min and detection was carried at 238 nm using a TUV detector. The retention times of metformin hydrochloride and nateglinide were found to be 1.28 1.71 min, respectively. Metformin hydrochloride and nateglinide were found to be linear over the concentration range of 125-750 and 15-90 μg/mL. The limit of detection and the limit of quantification for metformin hydrochloride were found to be 0.22 and 0.68 μg/mL, respectively, and, for nateglinide, 0.02 and 0.6 μg/mL, respectively. Developed method was validated as per ICH guidelines. The specificity of the method was confirmed by forced degradation study. The suggested method is suitable for determination of metformin hydrochloride and nateglinide in bulk and pharmaceutical dosage forms.

scholarly journals Photostability study of amlodipine besylate tablets packed in primary packaging

2021 ◽  
Vol 10 (1) ◽  
pp. 20-28
Author(s):  
Ivana Savić-Gajić ◽  
Ivan Savić ◽  
Predrag Sibinović ◽  
Valentina Marinković
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Amlodipine Besylate ◽  
Limit Of Quantification ◽  
First Order Kinetics ◽  
The Given

In this study, the modified stability-indicating RP-HPLC method was validated for quantitative analysis of amlodipine besylate in the presence of its impurity D (3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methylpyridine-3,5-dicarboxylate). The method was applied for the determination of an analyte in the tablets and irradiated samples packed in the primary packaging (Alu/PVC/PVDC blister packaging). The efficient chromatographic separation was achieved using a ZORBAX Eclipse XDB-C18 column (4.6×250 mm, 5 mm) with isocratic elution of mobile phase which consisted of acetonitrile:methanol:triethylamine solution (15:35:50, v/v/v) (pH 3.0). The flow rate of the mobile phase was 1 mL min-1, while the detection of amlodipine besylate was carried out at 273 nm. Amlodipine besylate and its impurity D were identified at the retention times of 16.529 min and 2.575 min, respectively. The linearity of the method with the coefficient of determination of 0.999 was confirmed in the concentration range of 10 - 75 µg mL-1 for amlodipine besylate. The limit of detection was 0.2 µg mL-1, while the limit of quantification was 0.66 µg mL-1. After UV and Vis radiation of the tablets packed in the primary packaging, the content of amlodipine besylate was reduced by 22.38% and 19.89%, respectively. The presence of new degradation products was not detected under the given chromatographic conditions. The photodegradation of amlodipine besylate followed pseudo-first-order kinetics. Based on the half-life of amlodipine besylate (38.4 days for UV radiation and 43.3 days for Vis radiation), it was concluded that amlodipine besylate in the tablets has satisfactory photostability after its packing in the Alu/PVC/PVDC blister packaging.

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

scholarly journals Reverse Phase Chiral HPLC Method for Enantiomeric Excess Determination of 2-Aminobutanamide

2019 ◽  
Vol 32 (1) ◽  
pp. 69-72
Author(s):  
T. Naga Jhansi ◽  
D. Pavan Kumar ◽  
Nagaraju Rajana ◽  
D. Jayadeep Kumar ◽  
G. Nageswara Rao
Keyword(s):  
Limit Of Detection ◽  
Enantiomeric Excess ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Perchloric Acid Solution ◽  
Column Temperature ◽  
Isomer Content

A reverse phase chiral HPLC method was developed for the determination of (R)-2-aminobutanamide isomer content in (S)-2-amino-butanamide key starting material for levetiracetam drug substance by using a CROWNPAK CR (+) column. Perchloric acid solution (0.05 %) was used as mobile phase and the flow rate was finalized as 0.3 mL/min. UV detection wavelength was 200 nm and column temperature was set as 15 ºC. The limit of detection and limit of quantification were 0.0002 mg/mL and 0.0005 mg/mL, respectively. The linearity calibration curve of (R)-2-aminobutanamide was shown good from the range of 0.0005 mg/mL to 0.004 mg/mL. The recovery of (R)-2-aminobutanamide isomer was between the range of 93 to 106 % in presence of (S)-2-aminobutanamide. The method was validated and found to be precise, accurate and robust. The method can be used for determination of (R)-2-aminobutanamide in presence of (S)-2-aminobutanamide, which is the key intermediate for preparation of levetiracetam. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods (1225).

scholarly journals Development and Validation of RP-Chiral HPLC Method for Determination of (R)-Enantiomer Excess Content in Efavirenz

2020 ◽  
Vol 32 (9) ◽  
pp. 2208-2212
Author(s):  
CH. RAMESH ◽  
DHARMASOTH RAMA DEVI DEVI ◽  
M.N.B. SRINIVAS ◽  
S. RADHA KRISHNA ◽  
NAGARAJU RAJANA ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Enantiomer Excess ◽  
Development And Validation ◽  
Methyl Phenyl

simple, specific, linear, accurate and precise reverse phase chiral HPLC method was developed for the separation of efavirenz enantiomers by using the Lux Amylose-2 column containing amylose tris(5-chloro-2-methyl phenyl carbamate) as a stationary phase. The mobile phase consists of 0.1 % formic acid in water and acetonitrile (55:45, v/v). The flow rate was kept at 1.0 mL/min and the detection wavelength used 252 nm and the column temperature was set at 25 ºC. The limit of detection was 0.01 mg/mL and the limit of quantification was 0.04 mg/mL. The linearity calibration curve of (R)-enantiomer was shown well from the range of 0.04 mg/mL to 0.4 mg/mL. The values of the correlation coefficient were 0.999 and 0.999 for (R)-enantiomer and (S)-efavirenz, respectively. The percentage recoveries of (R)-enantiomer from efavirenz drug substance were ranged from 93.5% to 107.5%. The results demonstrated that developed RP-chiral HPLC method was simple, precise, robust and applicable for the estimation of (R)-enantiomer in efavirenz API. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods <1225>.

A new stability indicating chiral RP-HPLC method for determination of degradation products in Meclizine Hydrochloride

2020 ◽  
Vol 16 ◽  
Author(s):  
Bryan Gowramma ◽  
Ramachandran Senthil Kumar ◽  
Kaviarasan Lakshmanan ◽  
Rajagopal Kalirajan ◽  
Subramanian Nainar Meyyanathan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Stress Conditions ◽  
Main Peak ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Degradation Behaviour ◽  
Stability Indicating

Background: An enantiomeric separation of stability-indicating high-performance liquid chromatographic method was developed and validated for the analysis of Meclizine enantiomers. The degradation behaviour of Meclizine Hydrochloride was investigated under different stress conditions recommended by International Conference on Harmonization (ICH). Experiment: Enantiomeric resolution of the drug and complete separation from its degradation products were successfully achieved on a Phenomenex® lux cellulose 1 C18 (250 mm × 4.6 mm i.d, 5 µm particle size) column, using UV detector at a wavelength of 230 nm, with mobile phase consisting of acetonitrile, 20mM ammonium bicarbonate at the ratio of 75:25 (v/v), and a flow rate of 1 mL/min. The drug was subjected to alkaline, acidic, neutral, oxidative and photolytic conditions in order to mimic stress conditions. Result: The degradation products were well resolved from main peak and proving the stability-indicating power of the method. The developed method provided linear responses within the concentration range 1-5 µg/mL, and regression analysis showed a correlation coefficient value (r2) of 0.999. The HPLC method was validated as per ICH guidelines with respect to specificity, precision, linearity and robustness. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.25 µg/mL and 1.00 µg/mL respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The method was highly selective, where degradation products and co formulated compounds did not interfere. The proposed method was successfully applied in pharmaceutical preparations.

Development and Validation of Stability-Indicating HPLC Method for Roflumilast and Related Substances

2013 ◽  
Vol 781-784 ◽  
pp. 68-71 ◽  
Author(s):  
Fang Tan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Limit Of Quantitation

A reversed phase HPLC method was developed and validated for analysis of roflumilast, its related substances and degradation products, using Ecosil C18 column (250×4.6 mm, 5 μm) with a flow rate of 1.0 ml/min and detection wavelength of 215nm. The mobile phase was a mixture of acetonitrile and 0.005mol·L-1ammonium dihydrogen phosphate buffer pH 3.5 in the ratio of 48:52 (v/v). The samples were analyzed using 20 μl injection volume and the column temperature was maintained at 30°C. The limit of detection and limit of quantitation were found to be 2.6 ng/ml and 8ng/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method is sensitive, specific, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds.

scholarly journals A simple isocratic RP-HPLC method for quality control of oseltamivir capsules

2012 ◽  
Vol 31 (2) ◽  
pp. 205
Author(s):  
Agim Ameti ◽  
Jasmina Slavkovska ◽  
Katerina Starkoska ◽  
Zorica Arsova-Sarafinovska
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Sample Treatment ◽  
Limit Of Quantification ◽  
Elution Time ◽  
Rp Hplc

A simple isocratic reversed-phase high performance liquid chromatographic (RP-HPLC) method was developed for determination of oseltamivir active pharmaceutical ingredient (API) in bulk drug and pharmaceuticals. The separation was achieved on a Purospher STAR® RP – 18e column with a mobile phase consisting of methanol- 0.02 mol l-1 phosphate buffer, pH 5, 50:50 (v/v). Chromatographic results demonstrated the specificity of the method for determination of oseltamivir in presence of degradation products generated in studies of forced decomposition. The limit of detection (LOD) and limit of quantification (LOQ) for oseltamivir phosphate were 0,0162 μg ml-1 and 0,0491 μg ml-1, respectively. The advantages of this method include simple sample treatment and short elution time (less than 6 min). Furthermore, using methanol instead of acetonitrile in a mobile phase composition considerably reduces the laboratory expenses, still retaining adequate sensitivity for routine analysis as well as for evaluation of potentially counterfeit Tamiflu® products. 

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