Validation of an analytical method based on QuEChERS and LC-MS/MS to quantify nine mycotoxins in plant-based milk

2021 ◽  
pp. 1-8
Author(s):  
L. Pinto ◽  
A. Santos ◽  
E. Vargas ◽  
F. Madureira ◽  
A. Faria ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Low Cost ◽  
Analytical Methodology ◽  
Relative Standard ◽  
Immunoaffinity Columns ◽  
Vegetable Milk ◽  
Aflatoxin B ◽  
Development And Validation ◽  
Proof Of Principle

Plant-based beverages (popularly known as vegetable milk) have become increasingly important in recent years. However, the nonexistence of information on mycotoxin contamination is noticeable. We herein describe the development and validation of an analytical methodology that employs QuEChERS and LC-MS/MS for the simultaneous determination of nine mycotoxins (aflatoxins B1, B2, G1, and G2, fumonisins B1 and B2, ochratoxin A, zearalenone, and citreoviridin) in seven types of vegetable milk (peanut, oat, rice, cashew, maize, soybean, and coconut). The method provided the following quantification limits, recoveries at the lowest validated concentration and relative standard deviations under repeatability conditions at the lowest validated concentration, respectively: aflatoxin B1 (0.023 μg/l, 84.98 and 9.23%); aflatoxin B2 (0.024 μg/, 93.00 and 4.85%); aflatoxin G1 (0.057 μg/l, 98.85 and 5.53%); aflatoxin G2 (0.031 μg/l, 96.64 and 4.08%); fumonisin B1 (2.166 μg/l, 75.55 and 16.78%); fumonisin B2 (1.105 μg/l, 70.47 and 11.89%); ochratoxin A (0.104 μg/l, 72.05 and 5.12%); zearalenone (8.093 μg/l, 107.10 and 6.37%); citreoviridin (1.305 μg/l, 97.25 and 7.28%). The method uses small amounts of samples, solvents, and other inexpensive reagents with no need for laborious clean-up and pre-concentration steps. Its attractive characteristics (simplicity, low cost compared to procedures that use immunoaffinity columns, and full compatibility with routine analyses) make it potentially valuable. As a proof-of-principle, the validated methodology was applied to seven commercial samples of different compositions showing that some were contaminated with aflatoxins and ochratoxin A.

Development and Validation of an Eco-Friendly and Low-Cost Method for the Quantification of Cefepime Hydrochloride in Powder for Injectable Solution Using Infrared (IR) Spectroscopy

2020 ◽  
Vol 16 (4) ◽  
pp. 456-464
Author(s):  
Danilo F. Rodrigues ◽  
Hérida R.N. Salgado
Keyword(s):  
Ir Spectroscopy ◽  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Potassium Bromide ◽  
Pharmaceutical Products ◽  
Injectable Formulation ◽  
Ich Guidelines ◽  
Lactam Ring ◽  
Development And Validation

Background: A simple, eco-friendly and low-cost Infrared (IR) method was developed and validated for the analysis of Cefepime Hydrochloride (CEF) in injectable formulation. Different from some other methods, which employ organic solvents in the analyses, this technique does not use these types of solvents, removing large impacts on the environment and risks to operators. Objective: This study aimed at developing and validating a green analytical method using IR spectroscopy for the determination of CEF in pharmaceutical preparations. Methods: The method was validated according to ICH guidelines and the quantification of CEF was performed in the spectral region absorbed at 1815-1745 cm-1 (stretching of the carbonyl group of β- lactam ring). Results: The validated method showed to be linear (r = 0.9999) in the range of 0.2 to 0.6 mg/pellet of potassium bromide, as well as for the parameters of selectivity, precision, accuracy, robustness and Limits of Detection (LOD) and Quantification (LOQ), being able to quantify the CEF in pharmaceutical preparations. The CEF content obtained by the IR method was 103.86%. Conclusion: Thus, the method developed may be an alternative in the quality control of CEF sample in lyophilized powder for injectable solution, as it presented important characteristics in the determination of the pharmaceutical products, with low analysis time and a decrease in the generation of toxic wastes to the environment.

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.

Development and validation of an analytical methodology for the determination of p,p′-DDT, p,p′-DDE and p,p′-DDD in fish oil pills

2007 ◽  
Vol 86 (2) ◽  
pp. 183-188 ◽  
Author(s):  
Juan José Berzas Nevado ◽  
Rosa Carmen Rodríguez Martín-Doimeadiós ◽  
Francisco Javier Guzmán Bernardo ◽  
Nuria Rodríguez Fariñas
Keyword(s):  
Fish Oil ◽  
Analytical Methodology ◽  
Development And Validation

scholarly journals Development and Validation of UV Spectrophotometric Method for the Determination of Cefuroxime Axetil in Bulk and Pharmaceutical Formulation

2013 ◽  
Vol 6 (1) ◽  
pp. 133-141 ◽  
Author(s):  
S. Binte Amir ◽  
M. A. Hossain ◽  
M. A. Mazid
Keyword(s):  
Spectrophotometric Method ◽  
Cost Effective ◽  
Cefuroxime Axetil ◽  
Pharmaceutical Formulation ◽  
Uv Spectrum ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Label Claim ◽  
Development And Validation

The present study was undertaken to develop and validate a simple, sensitive, accurate, precise and reproducible UV spectrophotometric method for cefuroxime axetil using methanol as solvent. In this method the simple UV spectrum of cefuroxime axetil in methanol was obtained which exhibits absorption maxima (?max) at 278 nm. The quantitative determination of the drug was carried out at 278 nm and Beer’s law was obeyed in the range of (0.80-3.60) µg/ml. The proposed method was applied to pharmaceutical formulation and percent amount of drug estimated (95.6% and 96%) was found in good agreement with the label claim. The developed method was successfully validated with respect to linearity, specificity, accuracy and precision. The method was shown linear in the mentioned concentrations having line equation y = 0.05x + 0.048 with correlation coefficient of 0.995. The recovery values for cefuroxime axetil ranged from 99.85-100.05. The relative standard deviation of six replicates of assay was less than 2%. The percent relative standard deviations of inter-day precision ranged between 1.45-1.92% and intra-day precision of cefuroxime axetil was 0.96-1.51%. Hence, proposed method was precise, accurate and cost effective.  Keywords: UV-Vis spectrophotometer; Method validation; Cefuroxime axetil; Recovery studies.  © 2013 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.   doi: http://dx.doi.org/10.3329/jsr.v6i1.14879 J. Sci. Res. 6 (1), 133-141 (2013)  

Development and validation of an LC–MS/MS method for the simultaneous determination of citrinin and ochratoxin a in a variety of feed and foodstuffs

2018 ◽  
Vol 1580 ◽  
pp. 100-109 ◽  
Author(s):  
Celine Meerpoel ◽  
Arnau Vidal ◽  
José Diana di Mavungu ◽  
Bart Huybrechts ◽  
Emmanuel K. Tangni ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Ochratoxin A ◽  
Development And Validation

scholarly journals Development and Validation of an UHPLC Method for Ostarine Determination in Dietary Supplements

2019 ◽  
Vol 65 (2) ◽  
pp. 49-54
Author(s):  
Amalia Miklos ◽  
Amelia Tero-Vescan ◽  
Lénárd Farczádi ◽  
Daniela-Lucia Muntean
Keyword(s):  
Quantitative Determination ◽  
Dietary Supplements ◽  
Low Cost ◽  
Reversed Phase ◽  
European Pharmacopoeia ◽  
Average Mass ◽  
7Th Edition ◽  
Development And Validation ◽  
Mg Content

AbstractObjective: The purpose of this study was to develop a low-cost, yet sensitive and precise UHPLC method for the quantitative determination of ostarine from dietary supplements (DS) for athletes. The analytical performance of the method was verified on a DS legally acquired from a specialized website for athletes. The uniformity of mass and content of the ostarine DS was also verified.Methods: For the quantitative determination of ostarine a UHPLC method was developed and validated. The separation was performed using a reversed-phase C18 column, using a mixture of 75% methanol: 25% formic acid 0.1% in isocratic elution, at a flow rate of 0.5 ml/min. The uniformity of mass and content of DS was performed following the methodology described in the European Pharmacopoeia 7th Edition.Results: The validated method was specific and linear on the concentration range of 1-25 µg/ml and was precise and accurate at all concentration levels, according to the official guidelines for validating analytical methods. An average mass of 510 mg content was obtained for the ostarine capsules, with an RSD of 2.41%. Regarding the uniformity of the content, an average of 4.65 mg ostarine/capsule was obtained with an RSD of 1.05%.Conclusions: The developed UHPLC method was suitable, rapid, sensitive and allowed quantitative determination of active substance content in a DS with ostarine (92.91% ostarine/capsule from 5 mg ostarine/capsule declared by the manufacturer).

scholarly journals Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

2009 ◽  
Vol 61 (4) ◽  
pp. 639-644 ◽  
Author(s):  
Gorica Vukovic ◽  
Snezana Pavlovic ◽  
M.S. Ristic
Keyword(s):  
Sample Preparation ◽  
Phosphoric Acid ◽  
Ochratoxin A ◽  
Chromatographic Determination ◽  
Liquid Extraction ◽  
Immunoaffinity Column ◽  
Maize Flour ◽  
Liquid Liquid Extraction ◽  
Immunoaffinity Columns

In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns). The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec?ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf?finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2) for the first method of sample preparation and 101% (%RSD = 2.2) for the second method. Values of LOQ for OTA were 0.25 and 1.00 ?g/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

scholarly journals Development and validation of spectrophotometric method for phenylephrine hydrochloride estimation in nasal drops formulations

2008 ◽  
Vol 27 (2) ◽  
pp. 149 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Vladimir Banković
Keyword(s):  
Standard Deviation ◽  
Sodium Hydroxide ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Development And Validation

Simple, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. Phenylephrine hydrochloride was estimated at 291 nm in 1 mol⋅dm-3 sodium hydroxide (pH 13.5). Beer’s law was obeyed in the concentration range of 10–100 μg⋅cm−3 (r2 = 0.9990) in the sodium hydroxide medium. The apparent molar absorptivity was found to be 1.63×103 dm3⋅mol−1⋅cm−1. The method was tested and validated for various parameters according to the ICH (International Conference on Harmonization) guidelines. The detection and quantitation limits were found to be 0.892 and 2.969 μg⋅cm−3, respectively. The proposed method was successfully applied for the determination of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 1 %), while being simple, cheap and less time consuming, and hence can be suitably applied for the estimation of phenylephrine hydrochloride in different dosage forms.

Determination of mean daily intakes of aflatoxin B1, aflatoxin M1, ochratoxin A, trichothecenes and fumonisins in 24-hour diets of children in the Netherlands

2009 ◽  
Vol 2 (4) ◽  
pp. 451-459 ◽  
Author(s):  
G. Bakker ◽  
E. Sizoo ◽  
A. Jekel ◽  
D.P. Pereboom-de Fauw ◽  
R. Schothorst ◽  
...  
Keyword(s):  
The Netherlands ◽  
Ochratoxin A ◽  
Daily Intake ◽  
Aflatoxin M1 ◽  
Limit Of Quantification ◽  
Diet Study ◽  
The Mean ◽  
Daily Intakes ◽  
Aflatoxin B

In 2006, a duplicate diet study of children's food was carried out in the Netherlands. Parents or guardians of 123 children collected duplicates of the 24-hour diets. Levels of aflatoxin M1, aflatoxin B1, ochratoxin A, trichothecenes and fumonisins were determined. Aflatoxin M1 was detectable in 10% of the samples, with all toxin levels below the limit of quantification. Aflatoxin B1 could be detected in 80% of the samples, while in 47% of all samples aflatoxin B1 was quantifiable. Ochratoxin A could be quantified in all samples. Deoxynivalenol was quantified in almost every sample, while T-2 and HT-2 toxins could only be quantified in 3.2% and 6.4% of the samples respectively. 15-acetyldeoxynivalenol was detected in 1.6% of the samples. Fumonisin B1 was detected in 28% of the samples and fumonisin B2 in a quarter of merely those samples where fumonisin B1 was detected. In 20% of the samples fumonisin B1 could be quantified and in a quarter of those samples fumonisin B2 could be quantified too. The analytical results were used to estimate levels of daily intake. Only the mean daily intake levels for aflatoxin B1, ochratoxin A, deoxynivalenol and fumonisins B1 and B2 could reliably be estimated. The values were 0.1, 4.1, 291 and 28 ng/kg bw/day respectively, all are well below the corresponding tolerable daily intakes. For aflatoxin B1 a tolerable intake does not exist, but the intake value for this mycotoxin was very low if compared to the value that would result from the intake of food, if it was contaminated with aflatoxin B1 at the EU regulatory limit, specified for baby food. The mean daily intakes of the mycotoxins determined in children's food in the Netherlands are low and implicate that there is no health risk for children due to exposure from the studied mycotoxins.

scholarly journals DEVELOPMENT AND VALIDATION OF UV-VISIBLE SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF DULOXETINE

2019 ◽  
pp. 27-31
Author(s):  
LIPSA SAMAL ◽  
AMARESH PRUSTY
Keyword(s):  
Spectrophotometric Method ◽  
Spectroscopic Method ◽  
Solvent System ◽  
Spectrophotometric Analysis ◽  
Thiophene Derivative ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Uv Visible ◽  
Development And Validation

Objective: The aim of the present work was to develop and validate a simple UV spectroscopic method for the determination of duloxetine, which is a thiophene derivative and a selective neurotransmitter reuptake inhibitor for serotonin, norepinephrine, and to lesser degree dopamine. Methods: The UV Spectrophotometric analysis was performed using Shimadzu UV-1800 and Shimadzu UV-1700 spectrophotometer by using solvent system acetonitrile and water in the ratio of 8:2. Detection was performed at a wavelength of 290 nm. Method validation was carried out according to ICH Q2R1 guidelines by taking the parameters linearity, accuracy, precision, ruggedness, and robustness, LOD and LOQ. Results: The UV Spectrophotometric method was found linear in the range of 10-50 μg/ml. The method was rugged and robust with % relative standard deviation less than 2. The extraction recoveries were found to be higher than 99% in all experimental conditions. Conclusion: Based upon the performance characteristics, the proposed method was found accurate, precise and rapid and suitable for the determination of Duloxetine for routine analysis.

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