scholarly journals Total Arsenic, Cadmium, and Lead Determination in Brazilian Rice Samples Using ICP-MS

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Lidiane Raquel Verola Mataveli ◽  
Márcia Liane Buzzo ◽  
Luciana Juncioni de Arauz ◽  
Maria de Fátima Henriques Carvalho ◽  
Edna Emy Kumagai Arakaki ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Limit Of Detection ◽  
Brown Rice ◽  
Total Arsenic ◽  
Limit Of Quantification ◽  
Rice Sample ◽  
Icp Ms ◽  
Validation Parameters ◽  
Rice Samples ◽  
Cadmium And Lead

This study is aimed at investigating a suitable method for rice sample preparation as well as validating and applying the method for monitoring the concentration of total arsenic, cadmium, and lead in rice by using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Various rice sample preparation procedures were evaluated. The analytical method was validated by measuring several parameters including limit of detection (LOD), limit of quantification (LOQ), linearity, relative bias, and repeatability. Regarding the sample preparation, recoveries of spiked samples were within the acceptable range from 89.3 to 98.2% for muffle furnace, 94.2 to 103.3% for heating block, 81.0 to 115.0% for hot plate, and 92.8 to 108.2% for microwave. Validation parameters showed that the method fits for its purpose, being the total arsenic, cadmium, and lead within the Brazilian Legislation limits. The method was applied for analyzing 37 rice samples (including polished, brown, and parboiled), consumed by the Brazilian population. The total arsenic, cadmium, and lead contents were lower than the established legislative values, except for total arsenic in one brown rice sample. This study indicated the need to establish monitoring programs for emphasizing the study on this type of cereal, aiming at promoting the Public Health.

Nanoparticulate Mycophenolic Acid Eye Drops - Analytical Validation of a High Performance Liquid Chromatography Assay and Stability Studies

2021 ◽  
Vol 09 ◽  
Author(s):  
Ali Al-Kulabi ◽  
Louis Gooden ◽  
Ijeoma F. Uchegbu
Keyword(s):  
Mycophenolic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Immunosuppressive Agent ◽  
Plate Count ◽  
Eye Drops ◽  
Limit Of Quantification ◽  
Drug Content ◽  
Relative Standard ◽  
Validation Parameters

Background: Mycophenolic acid (MPA), an immunosuppressive agent, is used orally to reduce corneal graft rejection. However its oral use is associated with gastrointestinal side effects. Objectives: To prepare MPA nanoparticle eye drops and a validated analytical method. Methods: Aqueous MPA eye drops were prepared by nanoencapsulation of MPA using Nanomerics MET (N-palamitoylN-monomethyl-N,N-dimethyl-N,N,N-trimethyl-6-O-glycolchitosan) at a MET, MPA ratio of 7.5: 1 g g-1 in the presence of glycerol (2.75% w/w). A validated MPA in-formulation drug substance assay was then developed. Results: MET-MPA formulations were prepared as well as a validated assay. Assay validation parameters for the analysis of MPA in the formulation were satisfactory [Plate count = 16458, Capacity Factor = 2.4, Tailing Factor = 1.02, linearity = 0.999 (0.016 – 0.5 mg mL-1 ), limit of detection = 0.056 mg mL-1 , limit of quantification = 0.17 mg mL-1 , accuracy = 98%, intraday and interday relative standard deviation = 0.45% and 4% respectively]. The candidate formulation (z - average mean = 66 ± 0.4 nm, polydispersity index = 0.12 ± 0.012, drug content = 1.14 ± 0.003 mg mL-1 , zeta potential = +8.5 ± 1.4 mV, pH = 7.4 ± 0.02, osmolarity = 309 ± 1.5 mOSm L-1 , viscosity = 1.04 ± 0.001 mPa.s) was then found to be stable for 14 days with respect to drug content at refrigeration, room and accelerated (40C )temperature and. All other formulation parameters were within the ocular comfort range. Conclusions: A validated assay (ICH and US FDA guidelines) for new MPA nanoparticle eye drops has been developed.

scholarly journals Development and Validation of a Simple Method for Routine Analysis of Ractopamine Hydrochloride in Raw Material and Feed Additives by HPLC

2009 ◽  
Vol 92 (3) ◽  
pp. 757-764 ◽  
Author(s):  
Ellen Figueiredo Freire ◽  
Keyller Bastos Borges ◽  
Hélio Tanimoto ◽  
Raquel Tassara Nogueira ◽  
Lucimara Cristiane Toso Bertolini ◽  
...  
Keyword(s):  
Quality Control ◽  
Limit Of Detection ◽  
Feed Additives ◽  
Raw Material ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Simple Method ◽  
Relative Standard ◽  
Validation Parameters ◽  
Ractopamine Hydrochloride

Abstract A simple method was optimized and validated for determination of ractopamine hydrochloride (RAC) in raw material and feed additives by HPLC for use in quality control in veterinary industries. The best-optimized conditions were a C8 column (250 4.6 mm id, 5.0 m particle size) at room temperature with acetonitrile100 mM sodium acetate buffer (pH 5.0; 75 + 25, v/v) mobile phase at a flow rate of 1.0 mL/min and UV detection at 275 nm. With these conditions, the retention time of RAC was around 5.2 min, and standard curves were linear in the concentration range of 160240 g/mL (correlation coefficient 0.999). Validation parameters, such as selectivity, linearity, limit of detection (ranged from 1.60 to 2.05 g/mL), limit of quantification (ranged from 4.26 to 6.84 g/mL), precision (relative standard deviation 1.87), accuracy (ranged from 96.97 to 100.54), and robustness, gave results within acceptable ranges. Therefore, the developed method can be successfully applied for the routine quality control analysis of raw material and feed additives.

scholarly journals NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF TELMISARTAN AND NEBIVOLOL HCL IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (9) ◽  
pp. 431 ◽  
Author(s):  
Heena Ar Shaikh ◽  
Vandana Jain
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.

scholarly journals ESTIMATION OF GUGGULSTERONE-Z IN GOKSHURADI GUGGULU USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (11) ◽  
pp. 204
Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Photodiode Array

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.

scholarly journals Methodological aspects concerning sampling and determination of total selenium and selenium species in geothermal waters

2020 ◽  
Vol 18 (1) ◽  
pp. 5-16 ◽  
Author(s):  
Piotr Rusiniak ◽  
Anna Ruszczyńska ◽  
Katarzyna Wątor ◽  
Ewa Bulska ◽  
Ewa Kmiecik
Keyword(s):  
Limit Of Detection ◽  
Selenium Concentration ◽  
Geothermal Water ◽  
Limit Of Quantification ◽  
Geothermal Waters ◽  
Selenium Species ◽  
Icp Ms ◽  
Significant Difference ◽  
Total Selenium

AbstractThe work presents the results of geothermal water sample analysis with respect to the determination of total selenium concentration. For this purpose, geothermal water (GT) samples were collected from three different intakes (GT-1, GT-2, GT-3) with similar temperatures of about 85°C. Tests were carried out to see if the methodology of sample preparation influenced total selenium concentration during analysis by inductively coupled plasma mass spectrometry (ICP-MS). Samples (raw and filtered) were preserved with nitric acid (HNO3) and mineralised in the laboratory. From the data obtained it was found that there is no significant difference between total selenium concentration in raw and filtered samples. Following mineralisation, the concentrations in the samples were below the limit of detection or limit of quantification. While different analytical steps or procedures are applied, the results of total selenium concentration can vary. Furthermore, high-performance liquid chromatography coupled with ICP-MS was used for the identification of selenium species. The results revealed that hexavalent selenium – Se(VI) – in the geothermal water was found only in samples collected from the GT-2 and GT-3 intakes.

scholarly journals Development and ICH Validation of a RP-HPLC-UV Method for the Quantification of Thimerosal in Topic Creams

2017 ◽  
Vol 60 (4) ◽  
Author(s):  
Guadalupe Pérez-Caballero ◽  
Nancy Muro-Hidalgo ◽  
Elvia Adriana Morales-Hipólito ◽  
Alma Villaseñor ◽  
Raquel López-Arellano
Keyword(s):  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Reversed Phase ◽  
Sample Treatment ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Quality Control Tool

A reversed phase high-performance liquid chromatography (RP-HPLC) method for determination of Thimerosal (TMS) in topical creams was optimized and validated according to the ICH guidelines which include accuracy, precision, selectivity, robustness, limit of detection (LOD), limit of quantification (LOQ), linearity and range. For topical creams, sample treatment is often an overwhelming step essentially due to its oily nature. For the first time a simple and robust extraction procedure for TMS using phosphate buffer (pH 5.5, 0.2M) was successfully developed. This method describes the TMS quantitation by HPLC in a topical product containing 0.01% fluocinolone acetonide (FLA) as the active molecule. The HPLC separation was achieved on a Column Symmetry® and a methanol: phosphate buffer (pH 2.5, 0.05M) 70:30 v/v mobile phase and wavelength 218 nm. Results from both standards and samples showed adequate validation parameters. Noteworthy, linearity was within the range 1.2 - 2.8 μg/mL. Additionally, robustness and TMS stability were established after sample extraction. The method provides an efficient and safe quality control tool for determination of TMS in topical creams.

scholarly journals Research Article on Development and Validation of RP-HPLC Method for Estimation of Canagliflozin

2019 ◽  
Vol 11 (02) ◽  
pp. 85-92
Author(s):  
Gudipally. Mounika ◽  
K. Bhavya Sri ◽  
R. Swethasri ◽  
M. Sumakanth
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Liquid Chromatography Method ◽  
Development And Validation

To develop an accurate, precise, specific high performance liquid chromatography method for quantification of Canagliflozin in bulk and dosage forms. A C18 column (250mm X 4.6mm; 5μm phenomenex) was used with mobile phase containing Acetonitrile-0.1% sodium acetate buffer (pH-4.6), (20:80) in isocratic mode. The flow rate maintained was 1.0ml/min and the U.V detector was operated at 291nm. The retention time of Canagliflozin was 3.307min and showed a good linearity in concentration range of 2-14μg/ml with correlation coefficient of 0.999. The average percent recovery was found to be 99.98%. The developed method follows validation parameters such as system suitability, linearity, precision, accuracy, limit of detection and limit of quantification and robustness as per ICH guidelinesQ2(R1). The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International conference on harmonization guidelines and successfully applied for bulk and pharmaceutical dosage form.

scholarly journals ANALYTICAL METHOD VALIDATION OF ICP-AES FOR ANALYSIS OF CADMIUM, CHROMIUM, CUPRUM, MANGAN AND NICKEL IN MILK

2019 ◽  
pp. 341-344
Author(s):  
DAVID ALEXANDER ◽  
Abdul Rohman
Keyword(s):  
Heavy Metals ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Official Method ◽  
Fast Method ◽  
Limit Of Quantification ◽  
Milk Products ◽  
Relative Standard ◽  
Validation Parameters

Objective: The aim of this research was to validate inductively coupled plasma-atomic emission spectroscopy (ICP-AES) for quantitative analysis of cadmium (Cd), chromium (Cr), cuprum (Cu), mangan (Mn) and nickel (Ni) in milk products. Methods: The heavy metals in milk were determined using ICP-AES at optimized wavelength. The method was validated by assessing several validation parameters which included linearity and range, accuracy, precision and sensitivity expressed by the limit of detection and limit of quantification. The validated method was then used for the analysis of milks commercially available. Results: ICP-AES for determination of Cd, Cr, Cu, Mn, and Ni was linear over a certain concentration range with a coefficient correlation value of>0.997. The limit of quantification values of Cd, Cr, Cu, Mn, and Ni were 0.0047; 0.0050; 0.0066; 0.0061; and 0.0169 µg/ml, respectively. The precision of analytical method exhibited relative standard deviation (RSD) values of 3.18%; 4.17%; 3.05%; 2.93%; and 4.47% during repeatability test and 5.28%; 5.06%; 3.67%; 3.67%; and 11.17% during intermediate precision of Cd, Cr, Cu, Mn, and Ni respectively. The recoveries of these metals assessed using standard addition method were 92.25; 90.88; 102.87; 94.50; and 86.85%, respectively. Conclusion: ICP-AES offered a reliable and fast method for the determination of heavy metals in milk products. The developed method could be proposed as an official method for determination of heavy metals in milk products.

scholarly journals ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF NORFLOXACIN PRESENT IN TASTE MASKED DRUG RESIN COMPLEX

2018 ◽  
Vol 11 (4) ◽  
pp. 244
Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.

Bioanalysis - Method Development, Validation, Sample Preparation, its Detection Techniques and its Application

2021 ◽  
pp. 297-305
Author(s):  
Seema R. Nikam ◽  
Amol S. Jagdale ◽  
Sahebrao S. Boraste ◽  
Shrikant B Patil
Keyword(s):  
Sample Preparation ◽  
Method Development ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Bioequivalence Study ◽  
Time Frame ◽  
Biological Drugs ◽  
Detection Techniques ◽  
Validation Parameters ◽  
Limit Of Quantitation

Quantitatively measurements of chemical and biological drugs and their metabolites in the biological sample. This used in clinical and non-clinical studies. Non clinical including Pharmacokinetic and Toxic kinetic study, and clinical including Bioavailability, Bioequivalence study. This are play significant role and help in improvement in technology and analytical methods. Recent years have witnessed the introduction of several high- quality review articles into the literature covering various scientific and technical aspects of bioanalysis. Method validation and development use for the purpose of suitability of method for their intended purpose, this are important in Drug Discovery and Development. It including a validation parameters are Accuracy, Precision, Range, Calibration Curve, Recovery, Limit of Detection, Limit of Quantitation, Specificity, Selectivity and Stability, Ruggedness. This applicable in bio analysis, FDA and EMA guidelines. There are 3 main Extraction techniques used in sample preparation in bioanalysis is precipitation, liquid –liquid extraction, solid phase extraction. Detection of analyte by using hyphenated and chromatographic techniques like LC-MS/MS, HPLC, GC-MS. This LC-MS/MS is commonly used in a bioanalysis. This bio analysis study used in Pharmaceutical, Biomedical research purpose. Many challenges in pharmaceutical industry that fulfill by the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality.

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