scholarly journals Method Development and Validation of Ion Chromatography Method for Determination of Free Sulfate in Fondaparinux Sodium Pre-Filled Syringe

2020 ◽  
Vol 32 (7) ◽  
pp. 1746-1750
Author(s):  
Kona S. Srinivas ◽  
Mahesh Kalva ◽  
Mallesh Changali ◽  
Narasimha S. L akka
Keyword(s):  
Ion Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Active Pharmaceutical Ingredient ◽  
Fondaparinux Sodium ◽  
Buffer Solution ◽  
Chromatography Method ◽  
Column Temperature

A simple ion chromatography method was developed for the quantitative determination of free sulfate in fondaparinux sodium pre-filled syringe for injection. Chromatographic separation was achieved on an anion-exchange resin column made of super macro porous polyvinyl benzyl ammonium polymer cross-linked with divinyl benzene (250 × 4.0 mm) with a mobile phase consisting of 60 mM carbonate buffer solution. Conductivity detector was employed with a flow rate of 0.7 mL min-1, injection volume of 100 μL and column temperature of 30 ºC. Retention time of sulfate (SO4 2−) was eluted at about 10.4 min. The developed method was validated in according to ICH Q2(R1) guideline and was found to be specific, precise, accurate, linear and robust. The precision was evaluated with six individual spiked samples of sulfate on Fondaparinux sodium for injection. The proposed method is linear (r2 > 0.9991) and accurate, mean recoveries were 99.2-117.8 % at 3 different levels (50-150%). The robustness was performed by changing the flow rate of mobile phase (0.7 ± 0.1mL min-1) and column temperature (30 ± 2 ºC). The proposed method is capable to determine free sulphate in fondaparinux sodium for injection in presence of excipients used in pharmaceutical formulation and also in its active pharmaceutical ingredient.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Lansoprazole in Presence of Related Substances by QbD Approach

2021 ◽  
pp. 138-150
Author(s):  
Sachin B. Gholve ◽  
Jaiprakash N. Sangshetti ◽  
Omprakash G. Bhusnure ◽  
Ram S. Sakhare ◽  
Pratap H. Bhosale ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Drug Substance ◽  
Gastric Ulcers ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Rp Hplc

A rapid specific RP-HPLC method has been developed for the determination of Lansoprazole impurities in the drug substance. The control of pharmaceutical impurities is currently a critical issue in the pharmaceutical industry. The International Council for Harmonization (ICH) has formulated a workable guideline regarding the control of impurities. The objective of the recent study was to develop and validate a HPLC method for the quantitative determination of process-related impurities of Lansoprazole in pharmaceutical drug substance. Lansoprazole, 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl] methyl]-sulfinyl]- 1H-benzimidazole is an proton pump inhibitor used in the management of gastric ulcers. Chromatographic identification of the impurities was carried out by response surface methodology, applying a three-level Box Behnken design with three center points. Three factors selected were a mobile phase, flow rate, column temperature. Evaluation of the main factor, their interaction, and the quadric effect on peak resolution were done on Waters Symmetry C8, 250 x 4.6mm, 5µm column is used for the development of the method. The mobile phase consists of buffer and acetonitrile. The flow rate of the mobile phase was 1.0 ml/min with gradient elution. The column temperature is ambient and the detection wavelength is 235 nm. The injection volume was 10 µL. The method was validated as per ICH guidelines for linearity in the range of 50-150 µg/ml and the LOD & LOQ values obtained were 0.437×10-4 and 0.1325×10-3 µg/ml respectively which specifies the method's sensitivity. The proposed method was successfully used to determine the Lansoprazole impurities in drug substances.

scholarly journals New ion-chromatography method for detection of chlorite, chlorate, and bromate in drinking water

2020 ◽  
Vol 2 (2) ◽  
pp. 49-55
Author(s):  
Iuliana Paun ◽  
Vasile Ion Iancu ◽  
Florentina Laura Chiriac ◽  
Nicoleta Vasilache ◽  
Florinela Pirvu ◽  
...  
Keyword(s):  
Drinking Water ◽  
Ion Chromatography ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Chromatography Method ◽  
Column Temperature ◽  
Drinking Waters ◽  
Target Analytes ◽  
Set Up

A direct ion chromatographic method for the determination of chlorite, chlorate, and bromate in the presence of fluoride, chloride, nitrate, nitrite, and bromide in treated drinking waters was described. Separation of target analytes was achieved using an AS19-HC analytical column (250 mm x 4 mm), AG 19- HC guard column (50 mm x 4 mm), and KOH 25 mmol/L as mobile phase. Inorganic analytes were eluted using a flow rate of 1 mL/min. The column temperature was set up and maintained at 300C. The analyte ions were quantified using a suppressed conductivity detector.

How to Analyze Ionic Liquid Anions? Investigation into the Application of Suppressed and Non-Suppressed Ion Chromatography

2008 ◽  
Vol 61 (6) ◽  
pp. 409 ◽  
Author(s):  
Piotr Stepnowski ◽  
Aleksandra Markowska
Keyword(s):  
Ionic Liquid ◽  
Ion Chromatography ◽  
Mobile Phase ◽  
Phthalic Acid ◽  
Time Frame ◽  
Buffer Solution ◽  
Bicarbonate Buffer ◽  
Reasonable Time Frame ◽  
Qualitative Determination

In the present study, two reliable and accurate methods have been developed for the quantitative and qualitative determination of ionic liquid anions based on suppressed and non-suppressed ion chromatography. They were applied to the separation and analysis of chloride, bromide, p-tosylate, tetrafluoroborate, hexafluorophosphate, dicyanamide, and bis(trifluoromethanesulfonyl)imide. In the non-suppressed mode, the influence of the concentration of phthalic acid, acetonitrile, and pH of the mobile phase on the retention and separation of analytes were investigated; 8 mM solution of phthalic acid with 20% v/v of acetonitrile (pH = 4) can be regarded as the optimal mobile phase in this separation mode. In the suppressed mode, various compositions of a carbonate/bicarbonate buffer solution with and without acetonitrile were also assessed; 3.2 mM Na2CO3/1 mM NaHCO3 and 25% acetonitrile were found to act as the optimal mobile phase. Under the analytical conditions developed, both methods provided very good separation and symmetrical peak shapes of all compounds within the reasonable time-frame of 30 min. The analytical performance parameters of both methods were good; however sensitivity will be further improved in future studies. Moreover, the suppressed separation mode was successfully applied to the analysis of tetrafluoroborate in a soil aquifer.

scholarly journals HPLC method for simultaneous determination of impurities and degradation products in Cardiazol

Pharmacia ◽  
2020 ◽  
Vol 67 (1) ◽  
pp. 29-37
Author(s):  
Iryna Drapak ◽  
Borys Zimenkovsky ◽  
Liudas Ivanauskas ◽  
Ivan Bezruk ◽  
Lina Perekhoda ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Degradation Products ◽  
Phase 1 ◽  
Simultaneous Detection ◽  
Hplc Method ◽  
Column Temperature ◽  
Degree Of Separation ◽  
Determination Of Impurities

Aim. The aim of study was to develop a simple and accurate procedure that could be applied for the determination of impurities and degradation products in cardiazol. Materials and methods. Separation in samples was carried out with Acquity H-class UPLC system (Waters, Milford, USA) equipped with Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) (Waters, Milford, USA). Xevo TQD triple quadrupole mass spectrometer detector (Waters Millford, USA) was used to obtain MS/MS data. Mobile phase A: 0.1% solution of trifluoroacetic acid R in water R; Mobile phase B: acetonitrile R. Samples were chromatographed in gradient mode (Table 1). Flow rate of the mobile phase: 1 ml / min. Column temperature: 30 °С. Detection: at 240 nm wavelength. Injection volume: 10 μl. Results. The retention time of the main substance is about 18.5 minutes. The order of the peak, the retention times and relative retention times: impurity B (12.04, 0.65); impurity А (18.5; 0.98); Cardiazol (18.87; 1.00). The LOD and LOQ values obtained were in the range of 30 ng/mL to 100 ng/mL and 80 ng/mL to 310 ng/mL respectively (with respect to sample concentration of 2 mg/ml). Linearity was established in the range of LOQ level to 0.2% having regression coefficients in the range of 0.9996 to 0.9999. The change in the temperature of the column affects the degree of separation of cardiazol and the impurity A, and thus, with a decrease of 5 ° C, the degree of separation is (1.06), while with increasing this index (3.43). When changing the flow rate of the mobile phase, the degree of separation changes in the following order, with a decrease to 0.9 ml / min separation (1.90), with an increase in speed to 1.1 ml / min (2.45). When the number of mobile phase B decreases by 5%, the degree of separation varies by (2.65), with an increase of 5% (1.82). In comparison with the chromatogram of the tested solution, the substance is not resistant to the action of peroxide, alkaline and acid decomposition. Conclusion. 1) HPLC method was developed and validated for the simultaneous detection and quantitation of impurities formed during the synthesis of cardiazol. 2) The method proved to be sensitive, selective, precise, linear, accurate and stability-indicating.

scholarly journals THE OPTIMIZATION OF HPLC FOR QUANTITATIVE ANALYSIS OF ACID ORANGE 7 AND SUDAN II IN COSMETIC PRODUCTS USING BOX BEHNKEN DESIGN

2019 ◽  
pp. 130-137 ◽  
Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Acid Orange 7 ◽  
Column Temperature ◽  
Box Behnken Design ◽  
Acid Orange

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 250 mm x 4.6 mm i.d.,5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.

Determination of Paeoniflorin and Paeonol in Houyinan Tablet by UPLC

2012 ◽  
Vol 581-582 ◽  
pp. 68-72
Author(s):  
Chu Qin Yu ◽  
Hua Qing Lin ◽  
Yue Han Hou ◽  
Zhong Feng Shi ◽  
Di Shi Lin
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Gradient Elution ◽  
The Other ◽  
Column Temperature ◽  
Average Recovery ◽  
Injection Volume

In this study, our purpose was to establish a UPLC method for the simultaneous determination of Paeoniflorin and Paeonol in Houyinan Tablet. The separation was performed on Acquity BEH C18 column(2.1mm×100mm,1.7μm), the mobile phase was acetonitrile-water with gradient elution at a flow rate of 0.2 mL•min-1, the detection wavelength was 230nm, the column temperature was 30°Cand the injection volume was 2μL. Paeoniflorin and Paeonol reached effective separation with the other components in this chromatographic conditions. Paeoniflorin and Paeonol were linear within the range of 0.0406~0.4064μg(r=0.9999) and 0.0426~0.4256μg (r=0.9999), respectively. The average recovery was 99.82% and 100.6%. The results of method validation indicated that the method was simple,quick,accurate, specific and less solvent consumption. It can be used for the quality control of Houyinan Tablet.

scholarly journals Experimental design approach for the development and validation of an enantiospecific RP-HPLC method for simultaneous determination of clopidogrel and related compounds

2008 ◽  
Vol 27 (1) ◽  
pp. 53 ◽  
Author(s):  
Rumenka Petkovska ◽  
Claus Cornett ◽  
Aneta Dimitrovska
Keyword(s):  
Experimental Design ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Hplc Method ◽  
System Response ◽  
Buffer Solution ◽  
Column Temperature ◽  
Rp Hplc ◽  
Related Compounds

An enantiospecific RP-HPLC method was developed and validated for the simultaneous determination of clopidogrel and four related compounds specified as impurities. Experimental design was applied during the method optimization (Full factorial 23 design) and robustness testing (Central Composite Face Centered design). Laboratory mixtures of clopidogrel and its impurities in a concentration ratio of 1: 5.0×10–4 were used as an investigation matrix. The three independent variables were the acetonitrile content in the mobile phase, pH of the mobile phase, and the column temperature. A Chromatographic Response Function (CRF) was used for estimation of the system response resolution (Rs). Separation was achieved using mobile phase composition of ACN: Buffer solution pH 6.5 (40:60 v/v) at 30 ºC. A CHIRAL-AGP 4.0 mm × 100 mm, 5.0 μm particle size column was used. The total time for chromatographic separation was approximately 10.0 min. The method was validated for its selectivity, linearity, precision, accuracy and robustness.

scholarly journals Design of experiments in optimization and validation of hydrophilic interaction liquid chromatography method for determination of amlodipine besylate and its impurities

2020 ◽  
Author(s):  
I. Kasagić-Vujanović ◽  
D. Knežević
Keyword(s):  
Design Of Experiments ◽  
Mobile Phase ◽  
Desirability Function ◽  
Hydrophilic Interaction ◽  
Amlodipine Besylate ◽  
Chromatography Method ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Validation Parameters

AbstractA new and rapid hydrophilic interaction liquid chromatographic method has been developed for the quantitative analysis of amlodipine besylate and its specific impurities (D, E, and F). For development of this method, a systematic approach which includes Design of Experiments methodology was applied. For the method optimization, Box–Behnken design and specific way Derringer's desirability function were applied. They provided identification of the optimal chromatographic conditions on the basis of obtained mathematical models and graphical procedures (three D graphs). The optimal chromatographic conditions were the analytical column ZORBAX NH2 (250 × 4.6 mm, 5 µm particle size); mobile phase consisted of acetonitrile-water phase (50 mM ammonium acetate, pH adjusted to 4.0 with glacial acetic acid) (90.5:9.5 v/v); column temperature 30 °C, mobile phase flow rate 1 mL min−1, wavelength of detection 230 nm. As other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of amlodipine besylate and its impurities in any laboratory under different circumstances has been proven.

scholarly journals RP-LC and TLC Densitometric Determination of Paracetamol and Pamabrom in Presence of Hazardous Impurity of Paracetamol and Application to Pharmaceuticals

2013 ◽  
Vol 8 ◽  
pp. ACI.S12349 ◽  
Author(s):  
Ola Mohamed El-Houssini
Keyword(s):  
High Performance Liquid Chromatography ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Thin Layer ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Column Temperature ◽  
Layer Chromatography

Two simple, accurate and reproducible methods were developed and validated for the simultaneous determination of paracetamol (PARA) and pamabrom (PAMB) in pure form and in tablets. The first method was based on reserved-phase high-performance liquid chromatography, on a Thermo Hypersil ODS column using methanol:0.01 M sodium hexane sulfonate:formic acid (67.5:212.5:1 v/v/v) as the mobile phase. The flow rate was 2 mL/min and the column temperature was adjusted to 35 °C. Quantification was achieved with UV detection at 277 nm over concentration range of 100-600 and 4-24 μg/mL, with mean percentage recoveries were found to be 99.90 ± 0.586 and 99.26 ± 0.901 for PARA and PAMB, respectively. The second method was based on thin-layer chromatography separation of PARA and PAMB followed by densitometric measurement of the spots at 254 nm and 277 nm for PARA and PAMB respectively. Separation was carried out on aluminum sheet of silica gel 60F254 using dichloromethane:methanol:glacial acetic acid (7.5:1:0.5 v/v/v) as the mobile phase over concentration range of 1-10 and 0.32-3.20 μg per spot, with mean percentage recovery of 100.52 ± 1.332 and 99.71 ± 1.478 for PARA and PAMB, respectively. The methods retained their accuracy in presence of up to 50% of P-aminophenol and could be successfully applied in tablets.

scholarly journals Development and Validation of a Precise Method for Determination of Benzalkonium Chloride (BKC) Preservative, in Pharmaceutical Formulation of Latanoprost Eye Drops

2010 ◽  
Vol 7 (1) ◽  
pp. 11-20 ◽  
Author(s):  
J. Mehta ◽  
K. Patidar ◽  
N. Vyas
Keyword(s):  
Flow Rate ◽  
Benzalkonium Chloride ◽  
Mobile Phase ◽  
Ophthalmic Solution ◽  
Pharmaceutical Formulation ◽  
Eye Drops ◽  
Intermediate Precision ◽  
Column Temperature ◽  
Validation Parameters

A simple and precise reversed phase high performance liquid chromatographic method has been developed and validated for the quantification of benzalkonium chloride (BKC) preservative in pharmaceutical formulation of latanoprost eye drops. The analyte was chromatographed on a Waters Spherisorb CN, (4.6×250 mm) column packed with particles of 5 μm. The mobile phase, optimized through an experimental design, was a 40:60 (v/v) mixture of potassium dihydrogen orthophosphate buffer (pH 5.5) and acetonitrile, pumped at a flow rate of 1.0 mL/min at maintaining column temperature at 30 °C. Maximum UV detection was achieved at 210 nm. The method was validated in terms of linearity, repeatability, intermediate precision and method accuracy. The method was shown to be robust, resisting to small deliberate changes in pH, flow rate and composition (organic ratio) of the mobile phase. The method was successfully applied for the determination of BKC in a pharmaceutical formulation of latanoprost ophthalmic solution without any interference from common excipients and drug substance. All the validation parameters were within the acceptance range, concordant to ICH guidelines.

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