scholarly journals An LLE Based LC- ESI MS/MS Analytical Method Development to Detect Azithromycin Residue in Water to Monitor Contamination Level of River and Fish Farm of Bangladesh

2021 ◽  
Author(s):  
Md Humayun Kabir ◽  
Sabina Yasmin ◽  
Salma Akter Mou ◽  
Bushra Parvin Upoma ◽  
Shamim Ahmed ◽  
...  
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Fish Farm ◽  
Contamination Level ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Esi Ms ◽  
Multiple Reaction Monitoring Mode

Abstract The aim of this study to development and validate an analytical method to determine the Azithromycin (AZN) residue in water approach to monitor the contamination level of river and fish farm water of Bangladesh. Azithromycin (AZN) was analyzed using liquid chromatography mass spectrometry (LC-ESI MS/MS). The chromatographic separations of analyte were performed using ZORBAX RRHD Eclipse Plus C18 (2.1×100 mm, particle size 1.8 µm) column and mobile phase was 0.1% formic acid in water and acetonitrile with 50:50. The analyte were detected in positive electron spray ionization mode with multiple reaction monitoring mode (MRM) with mass transition from 749.5 m/z to 591 m/z and 158 m/z as quantifier and qualifier ion respectively. Liquid-liquid extraction method was used for the extraction of AZN residues. The developed method was validated in terms of accuracy, precision, linearity and specificity. The analyte showed a good linear in the range of 0.1-100 µg/L. Three spiking levels (0.25, 0.5 and 1.25 µg/L) was performed for determining accuracy and precision. Recoveries and RSD were in the range of 96.6-101.5% and 3.5-6.3 respectively. The estimated limit of detection and limit of quantification was 0.017 and 0.05 µg/L respectively. Using the developed method, we analyzed 5 different rivers and 5 different fish farm samples. We found no azithromycin residue in rivers water, but we found in one fish farm water azithromycin residue 0.35±0.06 µg/L. The results indicate that we should be concern to use antibiotics in fish farm water in different ways.

scholarly journals Development and Validation of a Green Analytical Method for the Determination of Aspirin and Domperidone Bulk or Formulation Using UV and HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 49-56
Author(s):  
Sneha Jagnade ◽  
Pushpendra Soni ◽  
Lavakesh Kumar Omray
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Research Work ◽  
Ultra Violet ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation

The aim of present study was to investigate the development and validation of a green analytical method for the determination of aspirin and domperidone. Method Development and Validation for Estimation of Domperidone and Aspirin in bulk or formulation by using RP-HPLC. The RP-HPLC method was developed for estimation of Aspirin and Domperidone in synthetic mixture by isocratically using 10 mM KH2PO4: Acetonitrile (20:80) as mobile phase, Prontosil C-18 column (4.6 x 250 mm, 5μparticle size) column as stationary phase and chromatogram was recorded at 231 nm. Then developed method was validated by using various parameters such as, linearity, Range accuracy, precision repeatability, intermediate precision, robustness, limit of detection, limit of quantification. The proposed methods were found to be linear with correlation coefficient close to one. Precision was determined by repeatability, Intermediate precision and reproducibility of the drugs. The robustness of developed method was checked by changing in the deliberate variation in solvent. The result obtained shows the developed methods to be Cost effective, Rapid (Short retention time), Simple, Accurate (the value of SD and % RSD less than 2), Precise and can be successfully employed in the routine analysis of these drugs in bulk drug as well as in tablet dosage form. The Simplicity, Rapidly and Reproducibility of the proposed method completely fulfill the objective of this research work. Keywords: Asprin; Domperidone; HPLC; Ultra Violet; Validation

scholarly journals Determination of Pharmaceutical Residues by UPLC-MS/MS Method: Validation and Application on Surface Water and Hospital Wastewater

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Bui Van Hoi ◽  
Cam-Tu Vu ◽  
Lan-Anh Phung-Thi ◽  
Thao Thi Nguyen ◽  
Phuong Thanh Nguyen ◽  
...  
Keyword(s):  
Surface Water ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Hospital Wastewater ◽  
Esi Ms ◽  
Pharmaceutical Residues ◽  
Detection Frequency

In this study, an analytical method for the simultaneous determination of 7 major pharmaceutical residues in Vietnam, namely, carbamazepine, ciprofloxacin, ofloxacin, ketoprofen, paracetamol, sulfamethoxazole, and trimethoprim, in surface water and hospital wastewater has been developed. The method includes enrichment and clean-up steps by solid phase extraction using mix-mode cation exchange, followed by identification and quantification using an ultrahigh-performance liquid chromatography and tandem mass spectrometry and employing electrospray ionization (UPLC-ESI-MS/MS). Seven target compounds were separated on the reversed phase column and detected in multiple reaction monitoring (MRM) mode within 6 minutes. The present study also optimized the operating parameters of the mass spectrometer to achieve the highest analytical signals for all target compounds. All characteristic parameters of the analytical method were investigated, including linearity range, limit of detection, limit of quantification, precision, and accuracy. The important parameter in UPLC-ESI-MS/MS, matrix effect, was assessed and implemented via preextraction and postextraction spiking experiments. The overall recoveries of all target compounds were in the ranges from 55% to 109% and 56 % to 115% for surface water and hospital wastewater, respectively. Detection limits for surface water and hospital wastewater were 0.005–0.015 µg L−1 and 0.014–0.123 µg L−1, respectively. The sensitivity of the developed method was allowed for determination of target compounds at trace level in environmental water samples. The in-house validation of the developed method was performed by spiking experiment in both the surface water and hospital wastewater matrix. The method was then applied to analyze several surface water and hospital wastewater samples taken from West Lake and some hospitals in Vietnam, where the level of these pharmaceutical product residues was still missed. Sulfamethoxazole was present at a high detection frequency in both surface water (33% of analyzed samples) and hospital wastewater (81% of analyzed samples) samples.

Key Aspects of Analytical Method Development and Validation

2019 ◽  
Vol 31 (1) ◽  
pp. 32-39
Author(s):  
Suman Shrivastava ◽  
Pooja Deshpande ◽  
S. J. Daharwal
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Key Aspects ◽  
Development And Validation

Development of a method is crucial for discovery, development, and analysis of medicines in the pharmaceutical formulation. Method validation could also be thought to be one in all the foremost well-known areas in analytical chemistry as is reproduced within the substantial variety of articles submitted and presented in peer review journals every year. Validation of an analytical procedure is to demonstrate that it's appropriate for its intended purpose. Results from method validation are often wont to decide the quality, reliability and consistency of analytical results. Analytical methods need to be validated or revalidated. This review describes general approach towards validation process and validation parameters to be considered during validation of an analytical method. It also refers to various regulatory requirements like WHO, USFDA, EMEA, ICH, ISO/IEC. The parameters described here are according to ICH guidelines which include accuracy, precision, specificity, limit of detection, limit of quantification, linearity range and robustness.

scholarly journals BIO-ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF DECITABINE AND CEDAZURIDINE IN HUMAN PLASMA USING LC-MS/MS

2021 ◽  
pp. 257-262
Author(s):  
SAI PRUDHVI N. ◽  
VENKATESWARLU B. S. ◽  
KUMUDHAVALLI M. V. ◽  
MURUGANANTHAM V.
Keyword(s):  
Mass Spectrometry ◽  
Quality Control ◽  
Human Plasma ◽  
Method Development ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Validation Parameters

Objective: The present work aimed to develop a novel, reliable and accurate Liquid Chromatography-Mass Spectrometry/Mass spectrometry (LC-MS/MS) method for the simultaneous quantification of Decitabine and Cedazuridine a combined medication used for the treatment of chronic myelomonocytic leukemia in human plasma. Methods: Talazoparib drug is used as an internal standard in the study. Both the analytes and internal standard were isolated from 100 ml plasma samples by liquid-liquid extraction and then chromatographed on Zorbax SB-CN (4.6 mm×75 mm, 3.5 µm) column with a mobile phase consisting of 0.1 % ammonium formate and methanol in the ratio of 65:45 (v/v) pumped at 0.5 ml/min. The method had a chromatographic total run time of 5 min. Results: The developed method gave a symmetric peak at a retention time of 1.7 min for Decitabine, 2.2 min for Cedazuridine, 3.5 min for Talazoparib and satisfied all the peak properties as per USP guidelines. The mass spectral characterization of separated analytes in the LC method was performed using a mass detector operated at Multiple Reaction Monitoring mode with precursor-to-product ion transitions at m/z of 229 to m/z of 114 as MH+ion for Decitabine, m/z of 269 to m/z of 118 as MH+ion for Cedazuridine. A very sensitive limit of detection of 0.3 ng/ml was observed and showed a calibration curve linear over the concentration range of LLOQ (lower limit of quantification) to 500 ng/ml. The other validation parameters were found to have acceptable accuracy, precision, linearity, and selectivity. The mean extraction concentration was acceptable and very high for both the analytes in HQC (high-quality control concentration), MQC (medium quality control concentration) and LLOQ levels. The peak area response ratio of Decitabine and Cedazuridine with the internal standard in freeze-thaw, short term and long term stability studies was found to be acceptable confirms that the method is stable. Conclusion: It can be concluded that the proposed method is specific, accurate, and precise and could be used for the simultaneous estimation of Decitabine and Cedazuridine in human plasma.

scholarly journals A SELECTIVE AND SENSITIVE METHOD DEVELOPMENT AND VALIDATION BY LC-MS/MS APPROACH FOR TRACE LEVEL QUANTIFICATION OF POTENTIAL GENOTOXIC IMPURITY OF BOC EPOXIDE IN ATAZANAVIR SULPHATE DRUG SUBSTANCE

2017 ◽  
Vol 9 (9) ◽  
pp. 143
Author(s):  
Nelaturi Subbaiah ◽  
Gopireddy Venkata Subba Reddy
Keyword(s):  
Formic Acid ◽  
Method Development ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Ammonium Hydroxide ◽  
Active Pharmaceutical Ingredient ◽  
Accurate Method ◽  
Drug Substance ◽  
Internal Diameter ◽  
Limit Of Quantification

Objective: To develop and validate a selective, sensitive, rapid and accurate method using LC-MS/MS technique to achieve efficient separation between active pharmaceutical ingredient (Atazanavir sulphate) and genotoxic impurity (BOC epoxide).Methods: The quantification was carried out using the column puro sphere star RP 18 e (length 150 mm, internal diameter 4.6 mm, particle size 3.0 µm) with electrospray ionization in multiple reaction monitoring (MRM) detection mode. Eluent-A was 0.1% formic acid in water and eluent-B was 0.1% formic acid and 0.1% ammonium hydroxide solution (25%) in acetonitrile. The isocratic mode of elution was carried out for the elution of impurity with the shorter run time of 6 min. The flow rate was 1.0 ml/min and column oven temperature was maintained 25 °C.Results: The method was validated as per ICH guidelines and arrived the limit of detection and limit of quantification for the potential genotoxic impurity and found to be 0.2 ppm and 0.5 ppm. The developed method was found linear in the concentration range of 0.5 ppm to 6 ppm and accuracy results were within the range. Conclusion: The developed short span method found to be selective, sensitive, precise and accurate for the quantification of the BOC epoxide genotoxic impurity in atazanavir sulphate drug substance.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF NEW UFLC METHOD FOR DETERMINATION OF QUERCETIN IN ALCOHOLIC AND AQUEOUS EXTRACTS OF CAMELLIA SINENSIS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (08) ◽  
pp. 22-29
Author(s):  
T. N Kumar ◽  
◽  
B Gurupadayya ◽  
K Mruthunjaya ◽  
K. V Sairam
Keyword(s):  
Camellia Sinensis ◽  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Limit Of Quantification ◽  
Propyl Paraben ◽  
Specificity And Sensitivity ◽  
Method Accuracy

A precise, simple, responsive and feasible ultra-fast liquid chromatography (UFLC) method for novel analysis of quercetin in aqueous and alcoholic extracts of Camellia sinensis with internal standard has been developed. The analysis was carried out on a Phenomenax-C18 column (250 × 4.6mm, 5μm). Here, acetonitrile and orthophosporic acid of 0.1% V/V in water at a 60:40 ratio was used as the mobile phase and propyl paraben was used as the internal standard. The linearity range of quercetin was found to be between 1-25 µg/mL and retention times of quercetin and propyl paraben were found to be 3.3 and 5.6 min, respectively. In this developed method, accuracy and recovery values of quercetin were found to be good, ranging from 100 to 102% respectively. The proposed current novel analytical method was validated with respect to system suitability, linearity, limit of detection (LOD), precision and limit of quantification (LOQ), accuracy (recovery), specificity and sensitivity in respect to the ICH guidelines. This proposed method can be readily used for determination of quercetin in research institutes and quality control laboratories.

A NEW METHOD DEVELOPMENT AND VALIDATION FOR RELATED SUBSTANCES OF GRANISETRON IN ACTIVE PHARMA INGREDIENT BY HPLC

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (07) ◽  
pp. 52-59
Author(s):  
T. N Rao ◽  
◽  
Y. Prasanthi ◽  
Parvatamma Botsa ◽  
G. Kumara ◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Column Temperature ◽  
Related Substances ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation

A simple and inexpensive method was developed using high performance liquid chromatography with PDA detection for determination of granisetron hydrochloride and related impurities (2-methyl-N- [(1R,3r,5S)-9-methyl-9-azabicyclo[3.3.1]non-3-yl]-2H-indazole-3-carboxamide, 1-Methyl-N-[(1R,3r,5S)- 9-methyl-9-azabicyclo[3.3.1]non-3-yl]-1H-indazole-3-carboxamide hydrochloride, N-[(1R,3r,5S)-9- azabicyclo[3.3.1]non-3-yl]-1-methyl-1H-indazole-3-carboxamide and 1-methyl-1H-indazole-3-carboxylic acid. The chromatographic separations were achieved on (250×4.6 mm), 5.0 μm make: Waters, Symmetry Shield C8 column employing acetonitrile: 2% V/V H3PO4 in MilliQ water + 0.1% V/V hexylamine in water, 800:200 V/V (pH adjusted to 7.5 using triethylamine) mobile phase with isocratic programme. A flow rate of 1.5 mL/min was chosen. Four impurities were eluted within 20 minutes. The column temperature was maintained at 40°C and a detector wavelength of 300 nm was employed. The method was successfully validated by establishing system suitability, specificity, linearity, accuracy, limit of detection and limit of quantification.

Eco-Friendly Green Liquid Chromatographic Separations of a Novel Combination of Azelastine and Fluticasone in the Presence of their Pharmaceutical Dosage form Additives

2020 ◽  
Vol 16 (3) ◽  
pp. 277-286
Author(s):  
Amal A. El-Masry ◽  
Mohammed E. A. Hammouda ◽  
Dalia R. El-Wasseef ◽  
Saadia M. El-Ashry
Keyword(s):  
Lower Limit ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Uv Detection ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatographic

Background: The first highly sensitive, rapid and specific green microemulsion liquid chromatographic (MELC) method was established for the simultaneous estimation of fluticasone propionate (FLU) and azelastine HCl (AZL) in the presence of their pharmaceutical dosage form additives (phenylethyl alcohol (PEA) and benzalkonium chloride (BNZ)). Methods: The separation was performed on a C18 column using (o/w) microemulsion as a mobile phase which contains 0.2 M sodium dodecyl sulphate (SDS) as surfactant, 10% butanol as cosurfactant, 1% n-octanol as internal phase and 0.3% triethylamine (TEA) adjusted at pH 6 by 0.02 M phosphoric acid; with UV detection at 220 nm and programmed with flow rate of 1 mL/min. Results: The validation characteristics e.g. linearity, lower limit of quantification (LOQ), lower limit of detection (LOD), accuracy, precision, robustness and specificity were investigated. The proposed method showed linearity over the concentration range of (0.5-25 µg/mL) and (0.1-25 µg/mL) for FLU and AZL, respectively. Besides that, the method was adopted in a short chromatographic run with satisfactory resolution factors of (2.39, 3.78 and 6.74 between PEA/FLU, FLU/AZL and AZL/BNZ), respectively. The performed method was efficiently applied to pharmaceutical nasal spray with (mean recoveries ± SD) (99.80 ± 0.97) and (100.26 ± 0.96) for FLU and AZL, respectively. Conclusion: The suggested method was based on simultaneous determination of FLU and AZL in the presence of PEA and BNZ in pure form, laboratory synthetic mixture and its combined pharmaceutical dosage form using green MELC technique with UV detection. The proposed method appeared to be superior to the reported ones of being more sensitive and specific, as well as the separation was achieved with good performance in a relatively short analysis time (less than 7.5 min). Highly acceptable values of LOD and % RSD make this method superior to be used in quality control laboratories with of HPLC technique.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

scholarly journals A highly sensitive octopus-like azobenzene fluorescent probe for determination of abamectin B1 in apples

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Zhenlong Guo ◽  
YiFei Su ◽  
Kexin Li ◽  
MengYi Tang ◽  
Qiang Li ◽  
...  
Keyword(s):  
Fluorescent Probe ◽  
Limit Of Detection ◽  
Quantitative Detection ◽  
Fluorescence Signal ◽  
Ionization Mass ◽  
Limit Of Quantification ◽  
Visible Absorption ◽  
Esi Ms ◽  
Relative Standard ◽  
Ft Ir

AbstractThe development of detecting residual level of abamectin B1 in apples is of great importance to public health. Herein, we synthesized a octopus-like azobenzene fluorescent probe 1,3,5-tris (5′-[(E)-(p-phenoxyazo) diazenyl)] benzene-1,3-dicarboxylic acid) benzene (TPB) for preliminary detection of abamectin B1 in apples. The TPB molecule has been characterized by ultraviolet–visible absorption spectrometry, 1H-nuclear magnetic resonance, fourier-transform infrared (FT-IR), electrospray ionization mass spectroscopy (ESI-MS) and fluorescent spectra. A proper determination condition was optimized, with limit of detection and limit of quantification of 1.3 µg L−1 and 4.4 μg L−1, respectively. The mechanism of this probe to identify abamectin B1 was illustrated in terms of undergoing aromatic nucleophilic substitution, by comparing fluorescence changes, FT-IR and ESI-MS. Furthermore, a facile quantitative detection of the residual abamectin B1 in apples was achieved. Good reproducibility was present based on relative standard deviation of 2.2%. Six carboxyl recognition sites, three azo groups and unique fluorescence signal towards abamectin B1 of this fluorescent probe demonstrated reasonable sensitivity, specificity and selectivity. The results indicate that the octopus-like azobenzene fluorescent probe can be expected to be reliable for evaluating abamectin B1 in agricultural foods.

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