Quantitative determination of cyanoacetic acid content in teriflunomide drug substance by ion chromatography using conductivity detector

Abstract Background The current study focuses on the development and validation of an analytical method for quantifying cyanoacetic acid (CAA) in teriflunomide drug substance using a high-performance ion chromatography (IC) with cation suppressed conductivity detection (TFM). Water was used as the diluent for preparing the sample solution, which was injected into a standard chromatographic device with 250 mm, 4.0 mm ID, and 5.0 μm particle size Metrosep A Supp 5 Ion exchange column and a suppressed conductivity detector. At a flow rate of 0.6 mL min−1 and a temperature of 40 °C, the mobile phase was delivered in an isocratic mode. Results CAA and TFM had retention times of 12.78 and 15.82 min, respectively. CAA has a limit of detection (LOD) of 33 μg/g and a limit of quantification (LOQ) of 101 μg/g, respectively. For LOD and LOQ accuracy, the percentage RSD of CAA is 1.7 and 1.2, respectively. The average CAA recovery percentage was found to be between 98.6 and 100.1%. With a value of 0.9998, the calibration curve yielded an excellent linear correlation coefficient for CAA. According to the ICH guidelines, all verification parameters are within the range, indicating that the system is stable. Conclusion The elution time and run time in the currently developed ion chromatography analytical method have been reduced, demonstrating that the method is cost-effective and generally accepted, as well as simple and functional, and can be used in routine quality control tests in the industry.

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Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa100 ◽

2020 ◽

Author(s):

Murat Soyseven ◽

Rüstem Keçili ◽

Hassan Y Aboul-Enein ◽

Göksel Arli

Keyword(s):

Analytical Method ◽

High Performance ◽

Orthophosphoric Acid ◽

Limit Of Detection ◽

Detection System ◽

Active Pharmaceutical Ingredient ◽

Limit Of Quantification ◽

Column Temperature ◽

Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

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A Simple and Cost-Effective TLC-Densitometric Method for the Quantitative Determination of Acetylsalicylic Acid and Ascorbic Acid in Combined Effervescent Tablets

Molecules ◽

10.3390/molecules23123115 ◽

2018 ◽

Vol 23 (12) ◽

pp. 3115 ◽

Cited By ~ 2

Author(s):

Alina Pyka-Pająk ◽

Małgorzata Dołowy ◽

Wioletta Parys ◽

Katarzyna Bober ◽

Grażyna Janikowska

Keyword(s):

Ascorbic Acid ◽

Quantitative Determination ◽

Acetylsalicylic Acid ◽

High Performance ◽

Limit Of Detection ◽

Volume Ratio ◽

Cost Effective ◽

Pharmaceutical Formulations ◽

Limit Of Quantification

A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validated as per ICH guidelines by specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. Method validations indicate a good sensitivity with a low value of LOD and LOQ of both examined active substances. The linearity range was found to be 1.50–9.00 μg/spot and 1.50–13.50 μg/spot for acetylsalicylic and ascorbic acid, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of combined tablet formulation equal 97.1% and 101.6% in relation to the label claim that acetylsalicylic acid and ascorbic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine simultaneous analysis of acetylsalicylic acid and ascorbic acid in combined pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography in the quality control of above-mentioned substances, and it can be applied when HPLC or GC is not affordable in the laboratory.

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Simultaneous Identification and Quantification of Canrenone and 11-α-Hydroxy-Canrenone by LC-MS and HPLC-UVD

Journal of Biomedicine and Biotechnology ◽

10.1155/2011/917232 ◽

2011 ◽

Vol 2011 ◽

pp. 1-7 ◽

Cited By ~ 4

Author(s):

Da-Ming Huang ◽

Tian-Zhen Zhang ◽

Feng-Jie Cui ◽

Wen-Jing Sun ◽

Li-Ming Zhao ◽

...

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

Gradient Elution ◽

Limit Of Quantification ◽

Elution Time ◽

Ultraviolet Detector ◽

Simultaneous Identification ◽

Identification And Quantification

A procedure for simultaneous identification and quantification of canrenone and its biotransformed product 11-α-hydroxy-canrenone by high-performance liquid chromatography with ultraviolet detector (HPLC-UVD) and mass spectrometry (LC-MS) methods was proposed. The optimal determination variables on the HPLC-UVD or LC-MS coupled with a ZORBAX Eclipse XDB-C18 column (150 mm × 4.6 mm, 5 μm) were set as follows: detection wavelength of 280 nm, mobile phase of water and methanol gradient elution, temperature for the chromatographic column of 30°C, flow rate of mobile phase of 0.8 mL/min, sample injection volume of 5 μL, and elution time of 40 min. The MS conditions were set as follows: the flow rate of sheath gas, aux gas, and sweep gas were kept at 35 arb, 5 arb, and 0 arb, respectively. The temperature of capillary was held at 300°C, and capillary voltage was set at 30.00 V. Tube lens were performed at 100.00 V. The proposed method was validated by linearity ( ≥ 0.9910), average recovery (94.93%, RSD1.21%), precision (RSD ≤ 1.31%), limit of detection, and limit of quantification (LOD 0.1~0.12 mg/L, LOQ 0.5~0.67 mg/L), which proved to be affordable for simultaneously determining canrenone and its bio-transformed product 11-α-hydroxy-canrenone.

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Stability-indicating RP-UPLC Method for Determination of Vildagliptin in Drug Substance and Its Tablet Dosage Form

Journal of Pharmaceutical Research International ◽

10.9734/jpri/2021/v33i45a32726 ◽

2021 ◽

pp. 139-146

Author(s):

Kalyani Peluri ◽

S. Rajasekaran

Keyword(s):

Limit Of Detection ◽

Research Work ◽

Cost Effective ◽

Drug Substance ◽

Forced Degradation ◽

Limit Of Quantification ◽

Average Percentage ◽

Stability Indicating ◽

Degradation Studies

Aim: The foremost purpose of this research work is to diminish the analysis time and to establish cost effective method for estimation of Vildagliptin by RP-UPLC. Study Design: UPLC based Quantification studies. Place and Duration of Study: Department of Pharmacy, Bhagwant University, Ajmer, Rajasthan, Indiabetween June 2020 and August 2020. Methodology: A simple, responsive and precised RP-UPLC method with good robustness was developed and validated as per ICH for the analysis of Vildagliptin in drug substance and separation of degradants generated by different forced degradation conditions. Productive separation of Vildagliptin was attained by the use of Luna C18 column (100x2.6mm and 1.6µm) with a mobile phase composition of 0.1% v/v Trifluoroacetic acid and Acetonitrile in 80:20 v/v, which was pumped with 0.5 ml/min flow rate. The eluted substances were examined with PDA detector at 239nm. Stressed degradation studies were performed with proposed method to determine the percentage degradation of Vildagliptin. Results: The RT of Vildagliptin was observed at 1.56 min. The developed method was validated as per ICHQ2B and proved that the method was precise, sensitive, specific and accurate.The lowest concentration of limit of detection (0.05µg/ml) and limit of quantification(0.5µg/ml) of Vildagliptin make obvious about the sensitivity of the method. The correlation coefficient found to be 0.9997 for given range of linear concentrations. The calculated average percentage recoveries of Vildagliptin in spiked solutions were found to be in the range of 99.1-100.5. The calculated % RSD was determined to be less than 2. Determination of degradation of amount of Vildagliptin by forced degradation studies representing the stability indicating nature of the proposed method. Conclusion: The developed method said to be highly sensitive, accurate, specific and robust, therefore this method has high probability to adopt in pharmaceutical industry for regular analysis of Vildagliptin.

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RP-HPLC Method for the Determination and Quantification of Artesunate

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa037 ◽

2020 ◽

Vol 58 (8) ◽

pp. 695-699

Author(s):

Muhammad Asad Saeed ◽

Muhammad Tayyab Ansari ◽

Bashir Ahmad Ch ◽

Muhammad Zaman

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Cost Effective ◽

High Performance Liquid Chromatographic ◽

Hplc Method ◽

Limit Of Quantification ◽

Rp Hplc ◽

Ich Guidelines ◽

Average Retention Time ◽

Liquid Chromatographic

Abstract A simple, rapid and cost-effective reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed for the quantification of artesunate. C18 Promosil (ODS, 150 × 4.6 mm, 5 μm) column was used as stationary phase to separate the drug. Mobile phase comprised of ethanol: water (65:35) having pH 4.5 was run isocratically at a flow rate of 1 mL/min at 27°C. The method was validated according to ICH guidelines for linearity, precision, accuracy, robustness, specificity, limit of detection (LOD) and limit of quantification (LOQ). The method was found accurate, precise and robust with an average retention time of 4.509 min and 0.5357 %RSD. Good linearity was observed in the concentration range of 2–10 mg/ml with regression coefficient R2 value of 0.9995 and slope value of 369,928. Conclusively, as per ICH norms, the developed method was successfully validated and used for the quantification of artesunate in fast dissolving tablets (FDTs).

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Challenges of HPLC Method Development and Validation for the Assay of Bemotrizinol from Complex Matrix in Cosmeceutical Preparation

International Journal of Pharmaceutical Quality Assurance ◽

10.25258/ijpqa.11.3.2 ◽

2020 ◽

Vol 11 (03) ◽

pp. 310-316

Author(s):

Kallol S Jana ◽

Beduin Mahanti

Keyword(s):

Mobile Phase ◽

High Performance ◽

Method Development ◽

Limit Of Detection ◽

Linear Regression Analysis ◽

Cost Effective ◽

Analysis Data ◽

Hplc Method ◽

Limit Of Quantification ◽

Relative Standard

A simple high performance liquid chromatography (HPLC) method was developed for the assay of bemotrizinol (Tinosorb-S) from the complex pharmaceutical cosmetics matrix. Unlike the existing methods, the proposed mobile phase used in this method is very simple and excluding buffer. The use of buffer reducing column longevity and also a time-consuming process which increases the cost of analysis. To overcome all the referred problems, the present article was developed and validated as per International Council for Harmonization (ICH) guidelines. The reverse-phase chromatography was performed on Shimadzu model no. SPD-M10A VP with LC solution software, μBondapack (3.9 × 300 mm, 10-micron particle size) column with methanol (100%) as mobile phase at a flow rate 2.5 mL per minutes and UV detection at 254 nm. The retention time of bemotrizinol was found in 17.599 minutes, and the linear regression analysis data for the calibration plots showed a good linear relationship in the concentration range 70 to 130 μg/mL. The value of the correlation coefficient, slope, and intercept were 0.996, 7,715, and 15,320, respectively. The limit of quantification (LoQ) and limit of detection (LoD) were found to be 1.32 and 0.44, respectively. The relative standard deviation (RSD) for intra-day sample A 1.0858, sample B 0.8859, and inter-day sample A 0.9921, sample B 0.967 which were found to be lesser than 2%. The developed method was validated with regard to linearity, accuracy, precision, selectivity, and robustness, and the method was found to be simple, cost-effective, precise, accurate, linear, and specific for the successful identification and determination of bemotrizinol in pharmaceutical cosmetic preparation.

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ANALYTICAL METHOD BY HPLC-DAD ALLOWS QUANTIFICATION OF QUERCETIN MARKER IN STANDARDIZED EXTRACT OF ANADENANTHERA COLUBRINA VAR. CEBIL

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2017v9i8.16468 ◽

2017 ◽

Vol 9 (8) ◽

pp. 47

Author(s):

Valmir Gomes De Souza ◽

FabrÍcio Havy Dantas De Andrade ◽

Fabio Santos De Souza ◽

Rui Oliveira Macedo

Keyword(s):

Analytical Method ◽

High Performance ◽

Room Temperature ◽

Limit Of Detection ◽

Array Detector ◽

Diode Array Detector ◽

Limit Of Quantification ◽

Hydroalcoholic Extract ◽

Relative Standard ◽

Validation Parameters

Objective: The Anadenanthera colubrina (Vell.) Brennan var. cebil is a medicinal plant that has been used for the treatment of many diseases in the northeastern region of Brazil. This plant contains secondary metabolites such as quercetin, a flavonoid that is known by its antioxidant and anti-inflammatory effects. The aim of this work is to propose the validation of an analytical method using high-performance liquid chromatography with diode array detector (HPLC-DAD) for the quantification of quercetin and standardization of the hydroalcoholic extract (HAE) of A. colubrina.Methods: The A. colubrina extracts were prepared by the maceration process with powdered leaves at 20% weight: volume (w/v) and a hydroalcoholic solution at 50% volume: volume (v/v) for 120 h at room temperature. After pretreatment of the hydroalcoholic extract, the quercetin marker was used for quantification and proceeded to the evaluation of validation parameters for the method using HPLC-DAD.Results: The analytical method proved to be specific. Linear over the range 1.4–26.6 µg/ml, regression analysis showed a good correlation coefficient (R2= 0.999); the limit of detection (LOD) and the limit of quantification (LOQ) were 0.27 and 0.81 μg/ml respectively. The relative standard deviation (RSD) did not exceed 2.5% for precision. The proposed method was validated with an average recovery of 92.5–97.5%.Conclusion: The method was validated using HPLC-DAD, allowing the quantification of quercetin in the standardisation process of extracts and quality control of the herbal drug containing A. colubrina Phyto complex.

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Phytochemical Analysis of Twelve Marker Analytes in Sogunjung-tang Using a High-Performance Liquid Chromatography Method

Applied Sciences ◽

10.3390/app10238561 ◽

2020 ◽

Vol 10 (23) ◽

pp. 8561

Author(s):

Chang-Seob Seo ◽

Hyeun-Kyoo Shin

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Formic Acid ◽

Analytical Method ◽

High Performance ◽

Limit Of Detection ◽

Array Detector ◽

Phytochemical Analysis ◽

Limit Of Quantification ◽

Chromatography Method

Sogunjung-tang (SGJT) is a traditional herbal prescription that has been used in Korea for the treatment of abdominal pain since ancient times. In this study, an analytical method for the simultaneous quantification of 12 marker analytes (gallic acid (GA), albiflorin (ALB), paeoniflorin (PAE), liquiritin apioside (LIAP), liquiritin (PIQ), benzoic acid (BA), coumarin (COU), liquiritigenin (LIQG), cinnamic acid (CINA), benzoylpaeoniflorin (BPAE), cinnamaldehyde (CINAD), and glycyrrhizinic acid (GLYA)) for quality evaluation of SGJT was developed based on high-performance liquid chromatography (HPLC) combined with a photodiode array detector. A Waters SunFire reverse-phased C18 column was used for the chromatographic separation of the 12 marker analytes in SGJT using a two-mobile phases system consisting of 0.1% (v/v) aqueous formic acid and 0.1% (v/v) formic acid in acetonitrile. The developed analytical method was validated by assessment of linearity, limit of detection, limit of quantification, recovery, and precision. Using the developed and validated HPLC method, the 12 marker analytes were determined to be present in 0.10–32.83 mg/g in SGJT.

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SEPARATION AND DETERMINATION OF THE R-ISOMER OF ETODOLAC IN A BULK DRUG SUBSTANCE BY NORMAL-PHASE LIQUID CHROMATOGRAPHY

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2016.v9i6.14597 ◽

2016 ◽

Vol 9 (6) ◽

pp. 327

Author(s):

Appasaheb Bajirao Lawande

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Analytical Method ◽

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

Normal Phase ◽

Limit Of Quantification ◽

Bulk Drug

ABSTRACT Objective: The objective of the this work is to develop and validate a novel, simple,rapid and reliable analytical method for separation and determination of R-isomer impurity in Etodolac bulk drug material by normal-phase high-performance liquid chromatography as per International Conference on Harmonization guidelines. Methods: The Etodolac R- isomer and S-isomer were separated on a Chiralcel OD-H (150 x 4.0 mm, 5 micron) column by using Ethanol : n-Hexane:Trifluoroacetic acid (50:50:0.1 v/v.) mobile phase with equipped detector at wavelength 225 nm and 25 °C column oven temperature. The resolution between R-isomer and S-isomer were more than two recorded on chromatogram. The specified method was developed and validated for various parameters like reproducibility, limit of detection, limit of quantification, linearity and range, robustness, solution stability and mobile phase stability according to the International Conference on Harmonization (ICH) guidelines. Results: Linearity were found for Etodolac R-isomer over the concentration range of 600–6000 ng/ml, with the linear regression (Correlation coefficient R = 0.998) and proved to be robust. Limit of detection and limit of quantification of Etodolac R-isomer was found to be 200 and 600 ng/ml. The retention time of R-isomer was considered to be 2.8 min. The percentage recovery of Etodolac R-isomer has been ranged from 97.0 to 102.0 in bulk drug material sample. The proposed analytical method has been found to be suitable, precise,reliable and accurate for the separation and quantitative determination of Etodolac R-isomer in bulk drug sample. Conclusion: A novel, speedy, accurate, precise, reliable and rugged analytical method has been developed and validated for normal phase high performance liquid chromatography to determine R-isomer impurity in Etodolac bulk drugs material as per ICH guideline. Keywords: Etodolac, HPLC, Known Impurity. Normal Phase, Validation.

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Development of a QuEChERS-Based UHPLC-MS/MS Method for Simultaneous Determination of Six Alternaria Toxins in Grapes

Toxins ◽

10.3390/toxins11020087 ◽

2019 ◽

Vol 11 (2) ◽

pp. 87 ◽

Cited By ~ 8

Author(s):

Wenbo Guo ◽

Kai Fan ◽

Dongxia Nie ◽

Jiajia Meng ◽

Qingwen Huang ◽

...

Keyword(s):

Simultaneous Determination ◽

Analytical Method ◽

High Performance ◽

Limit Of Detection ◽

Safe Procedure ◽

Alternariol Monomethyl Ether ◽

Limit Of Quantification ◽

Alternaria Toxins ◽

Relative Standard

A simple and reliable analytical method for the simultaneous determination of alternariol (AOH), altenuene (ALT), tentoxin (TEN), altenusin (ALS), tenuazonic acid (TeA), and alternariol monomethyl ether (AME) in grapes was developed by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with the extraction by acetonitrile and purification by sodium chloride (0.5 g) and anhydrous magnesium sulfate (0.5 g) was established to recover the six Alternaria toxins. After validation by determining the linearity (R2 > 0.99), recovery (77.8–101.6%), sensitivity (limit of detection in the range of 0.03–0.21 μg kg−1, and limit of quantification in the range of 0.09–0.48 μg kg−1), and precision (relative standard deviation (RSD) ≤ 12.9%), the analytical method was successfully applied to reveal the contamination state of Alternaria toxins in grapes. Among 56 grape samples, 40 (incidence of 71.4%) were contaminated with Alternaria toxins. TEN was the most frequently found mycotoxin (37.5%), with a concentration range of 0.10–1.64 μg kg−1, followed by TeA (28.6%) and AOH (26.8%). ALT (10.7%), AME (3.6%), and ALS (5.4%) were also detected in some samples. To the best of our knowledge, this is the first report about the Alternaria toxins contamination in grapes in China.

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