scholarly journals Determination of Ethanol Content in Kombucha Using Headspace Gas Chromatography with Mass Spectrometry Detection: Single-Laboratory Validation

2020 ◽  
Author(s):  
Michael Chan ◽  
Hong Sy ◽  
Jamie Finley ◽  
Jake Robertson ◽  
Paula N Brown
Keyword(s):  
Dynamic Range ◽  
Limit Of Detection ◽  
Alcoholic Beverage ◽  
The United States ◽  
Limit Of Quantification ◽  
Method Performance ◽  
Potential Health ◽  
Headspace Gas ◽  
Gas Chromatographic Method

Abstract Background Kombucha is a fermented beverage made with tea, sugar, and a symbiotic colony of bacteria and yeast that is usually marketed as a non-alcoholic beverage. Products must contain <0.5% and <1.1% alcohol by volume in the United States and Canada respectively to be classified as non-alcoholic products. Prior studies have found that Kombucha beverages can become very acidic and may contain levels of alcohol above 1% which can be a potential health risk to children and the developing fetus during pregnancy. Objective Given the public safety concerns and legal requirements associated with the level of alcohol within Kombucha beverages, there is a need for accurate and reliable methods. Herein we describe the validation of a sensitive, rapid, and simple Headspace Gas Chromatographic method with mass spectrometric detection for determining ethanol in Kombucha. Methods Method performance characteristics measured included linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) as per AOAC International guideline Appendix K Part 1. Performance was evaluated against the AOAC Standard Method Performance Requirements 2016.001 for determination of ethanol in Kombucha. Results The linear dynamic range for this method was confirmed over the range of 0.025 to 2.47% ABV. The LOD and LOQ were determined to be 0.0002% and 0.002% ABV, respectively. With a spike recovery of 102% for accuracy and precision of RSDr ≤ 4% the method met the SMPR requirements within the analytical range. Conclusions The results of this validation study demonstrated the method is fit for the purpose of quantifying ethanol in Kombucha and is suitable for rapid and easy integration by laboratories to ensure that regulatory requirements are met.

Gas Chromatographic Determination of Polychlorinated Biphenyls in Mussels from Galicia, Spain

1994 ◽  
Vol 77 (4) ◽  
pp. 985-988 ◽  
Author(s):  
Elena Alvarez Piñeiro ◽  
Jesus Simal Lozano ◽  
Asuncion Lage Yusty
Keyword(s):  
Environmental Protection Agency ◽  
Mytilus Galloprovincialis ◽  
Capillary Column ◽  
Polychlorinated Biphenyl ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Method Performance ◽  
The Mean ◽  
Gas Chromatographic Method

Abstract We have modified a standard capillary column gas chromatographic method (U.S. Environmental Protection Agency No. 505) for the determination of polychlorinated biphenyl (PCB) residues and applied the technique to mussels (Mytilus galloprovincialis) from Galicia, Spain. During the purification step, SepPak Florisil minicolumns are used instead of conventional columns. Method performance is good (limit of detection, 0.032 μg/kg; recovery, 99%; method precision as coefficient of variation among 10 samples, 2.5%), and compared with the standard method, less eluant is required and analysis is faster. The mean PCB content of 107 mussels collected from various points on the coast of Galicia was 113 μg/kg.

scholarly journals Determination of Ethanol Concentration in Kombucha Beverages: Single-Laboratory Validation of an Enzymatic Method, First Action Method 2019.08

2020 ◽  
Author(s):  
Ruth Ivory ◽  
Elaine Delaney ◽  
David Mangan ◽  
Barry V McCleary
Keyword(s):  
Fruit Juice ◽  
Limit Of Detection ◽  
Alcoholic Beverage ◽  
Limit Of Quantification ◽  
Easy Method ◽  
Test Kit ◽  
High Possibility ◽  
Single Laboratory ◽  
Low Alcohol

Abstract Kombucha is a fermented, lightly effervescent sweetened black or green tea drink. It is marketed as a functional beverage based on its proposed health benefits. Kombucha is produced by fermenting tea using a “symbiotic colony of bacteria and yeast” (SCOBY). Kombucha is marketed as a non-alcoholic beverage, however due to the production process employed, there is a high possibility that the Kombucha products will contain low levels of ethanol. Kombucha is sold in a raw and unpasteurized form and, if kept at temperatures above 4 °C, the possibility exists that it will continue to ferment, producing ethanol. This possibility of continued fermentation may lead to an increase in ethanol content from levels below 0.5%ABV at time of production to higher levels at time of consumption. Thus, there is a potential for levels rising to greater than 0.5%ABV, the threshold for certification as a non-alcoholic beverage. It is essential that Kombucha manufacturers have the capacity to accurately and quickly test for ethanol in their products.  The Ethanol Assay Kit is an enzymatic test kit developed by Megazyme for the determination of ethanol in a variety of samples. The kit has been validated in a single laboratory for use with Kombucha fermented drinks, fruit juices, and low-alcohol beer samples. The commercially available Ethanol Assay Kit (Megazyme catalogue no. K-ETOH) contains all components required for the analysis. Quantification is based on the oxidation of ethanol to acetaldehyde by alcohol dehydrogenase and further oxidation of acetaldehyde by acetaldehyde dehydrogenase with conversion of NAD+ to NADH. The single laboratory validation (SLV) outlined in this document was performed on a sample set of eight different commercial Kombucha products purchased in Ireland, a set of five Cerilliant aqueous ethanol solutions, two BCR low-alcohol beer reference materials, two alcohol-free beer samples, and two fruit juice samples against SMPR 2016.001 (1). Parameters examined during the validation included Working range, Selectivity, Limit of Detection (LOD), Limit of Quantification (LOQ), Trueness (bias), Precision (reproducibility and repeatability), Robustness, and Stability. The Ethanol Assay is a robust, quick and easy method for the measurement of ethanol in Kombucha. Our data suggests this method is also reliable for similar matrices, such as low-alcohol beer and fruit juice. The assay meets all requirements set out in in AOAC SMPR 2016.001.

scholarly journals Development and Validation of a Headspace Gas Chromatographic (HS-GC) Method for Determination of Residual Solvents in Nitazoxanide API

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 1719-1727
Author(s):  
Rajesh Kumar Chawla ◽  
Koteswara Rao G S N ◽  
Umasankar Kulandaivelu ◽  
Siva Prasad Panda ◽  
Rajasekhar Reddy Alavala
Keyword(s):  
Limit Of Detection ◽  
Dimethyl Formamide ◽  
Limit Of Quantification ◽  
Residual Solvents ◽  
Pharmaceutical Ingredients ◽  
Quality Control Laboratory ◽  
Ich Guidelines ◽  
Headspace Gas ◽  
Development And Validation

Controlling residual solvents in the drug substances or active pharmaceutical ingredients (API) is mandatory to the specified limits as per the International Conference on Harmonisation (ICH) Q3C guidelines. Residual solvents in pharmaceuticals are mostly determined by Gas Chromatography with Headspace. A simple and sensitive headspace gas chromatographic (HS-GC) method has been developed for the determination of Acetone, Dichloromethane and Cyclohexane in Nitazoxanide API. The separation of analytes was achieved with DB – 624 (30 m length, 0.53 mm inner diameter and 3.0 μm in film thickness) capillary column. Dimethyl formamide was used as a diluent. Nitrogen was used as carrier gas with 3.0 mL/minutes and Flame ionisation detector (FID) for detecting analytes. The oven temperature was set at 60°C for 5 minutes at initial and programmed at a rate of 20°C per minute to a final temperature of 240°C for 2 minutes. Run time was 16 minutes, and total GC cycle time was 25 minutes. The spilt ratio used as 1:20 to get optimum peak response. The developed method was validated as per the ICH guidelines for specificity, accuracy, precision, linearity, range, the limit of detection, the limit of quantification and robustness. The results of validation were indicated no interference, good recoveries, precise, linear, rugged and robust method, suitable for the determination of residual solvents in Nitazoxanide API for research and routine quality control laboratory.

scholarly journals DETERMINATION OF RESIDUAL DIMETHYL SULFATE IN METHOXSALEN DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION WITH STATIC HEADSPACE GAS CHROMATOGRAPHY

2018 ◽  
Vol 10 (8) ◽  
pp. 84
Author(s):  
Ajit Anerao ◽  
Bhushan Patil ◽  
Nitin Pradhan
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Sulfate ◽  
Drug Substance ◽  
Headspace Gas Chromatography ◽  
Limit Of Quantification ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas

Objective: Dimethyl sulfate has been highlighted as potential genotoxic and carcinogenic impurity. A sensitive Headspace gas chromatography (HS-GC) method with pre-column derivatization was developed and validated for the determination of dimethyl sulfate impurity in methoxsalen active pharmaceutical ingredient.Methods: HS-GC method on the column Agilent DB-5, 30m X 0.53 mm, film thickness 1.5 µm, with flame ionization detector (FID) was used. Derivatization reagent concentration, time of reaction and pH of the solution were optimized during method development. This analytical method was evaluated by performing method validation as per ICH guideline.Results: The proposed method was specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.5 μg/ml to 3.0 μg/ml and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) 2.0 μg/g and 5.0 μg/g respectively. Accuracy was observed within 98.1%–104.5%.Conclusion: The developed method was demonstrated to be accurate, robust and sensitive for the determination of dimethyl sulfate impurity in methoxsalen drug substance.

scholarly journals Spectrophotometric determination of diclofenac in pharmaceutical preparations assisted by microwave oven

2005 ◽  
Vol 30 (1) ◽  
pp. 29-36 ◽  
Author(s):  
E. G. Ciapina ◽  
A. O. Santini ◽  
P. L. Weinert ◽  
M. A. Gotardo ◽  
H. R. Pezza ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Low Cost ◽  
Standard Procedure ◽  
Pharmaceutical Preparations ◽  
Magnesium Stearate ◽  
The United States ◽  
Molar Absorptivity ◽  
Heating Time ◽  
Limit Of Quantification

In this work, an effective and low-cost method for the determination of sodium or potassium diclofenac is proposed in its pure form and in their pharmaceutical preparations. The method is based on the reaction between diclofenac and tetrachloro-p-benzoquinone (p-chloranil), in methanol medium. This reaction was accelerated by irradiating of reactional mixture with microwave energy (1100 W) during 27 seconds, producing a charge transfer complex with a maximum absorption at 535 nm. The optimal reaction conditions values such as reagent concentration, heating time and stability of the reaction product were determined. Beer's law is obeyed in a concentration range from of 1.25x10-4 to 2.00x10-3 mol l-1 with a correlation coefficient of 0.9993 and molar absorptivity of 0.49 x10³ l mol-1 cm-1. The limit of detection (LOD) was 1.35x10-5 mol l-1 and the limit of quantification (LOQ) was 4.49x10-5 mol l-1. In the presence of the common excipients, such as glucose, lactose, talc, starch, magnesium stearate, sodium sulphite, titanium dioxide, polyethyleneglycol, polyvinylpirrolidone, mannitol and benzilic alcohol no interferences were observed. The analytical results obtained by applying the proposed method compare very favorably with those given by the United States Pharmacopeia standard procedure. Recoveries of diclofenac from various pharmaceutical preparations were within 95.9% to 103.3%, with standard deviations ranging from 0.2% to 1.8%.

Determination of epinephrine in human serum using a Pt electrode modified by polyaniline–poly(3-methylthiophene)–poly(3,3′-diaminobenzidine)

2015 ◽  
Vol 93 (11) ◽  
pp. 1239-1244 ◽  
Author(s):  
Emine Ülker ◽  
Muammer Kavanoz
Keyword(s):  
Human Serum ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Oxidation Potential ◽  
Serum Samples ◽  
Pt Electrode ◽  
Limit Of Quantification ◽  
Amperometric Determination ◽  
Best Response

A Pt electrode modified by polyaniline–poly(3-methylthiophene)–poly(3,3′-diaminobenzidine) was used for amperometric determination of epinephrine in a solution of NaHSO4/Na2SO4 (pH 2.0). For these studies, potentials between 0.40 and 0.50 V were applied, and the best response was obtained at 0.45 V. The limit of detection, limit of quantification, and the linear dynamic range were 1.23 × 10−4, 4.10 × 10−4, and 4.10 × 10−4 to 100.0 mmol L−1, respectively. These results were compared with determinations using Pt electrodes that were coated and uncoated with homopolymers. To check the accuracy of the developed method and the matrices interference, determination of epinephrine was performed in human serum samples using this modified electrode. The epinephrine concentrations were adjusted to 1.0 and 5.0 mmol L−1, and recovery values were calculated as 100.4% and 96.8%, respectively. It is significant that the determination of epinephrine was carried out at a lower potential (0.45 V) than the oxidation potential of epinephrine (0.65 V) without any matrix effect.

IN VITRO ANALYTICAL EVALUATION OF NITROSAMINE – A CARCINOGENIC IMPURITIES IN OLMESARTAN MEDOXIMIL BY GC MS/MS METHOD

2020 ◽  
pp. 89-94
Author(s):  
NDVR SARADHI ◽  
K KALYAN KUMAR ◽  
M VENKATA REDDY
Keyword(s):  
Mass Spectrometer ◽  
Method Development ◽  
Limit Of Detection ◽  
The United States ◽  
Mass Analyzer ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Tandem Mass Spectrometer

Objective: A simple and sensitive method development and validation for the simultaneous determination of the N-nitrosamine dimethylamine (NDMA) and N Nitrosamine diethylamine (NDEA) in Olmesartan medoxomil (OLM) API and formulations by a tandem mass spectrometer (GC-MS/MS). Methods: Gas chromatography with a programmed oven temperature controller, Elite Wax (30 m × 0.25 mm × 0.5 μm) column, Helium as carrier gas and hyphenated to the tandem mass spectrometer powered with triple quadrupole mass analyzer, and photomultiplier tube detector. The method was validated as per the United States Food and Drug Administration (USFDA) guidelines. Results: With the selected GC-MS/MS conditions, the NDMA and NDEA 0.08 μg/ml (80 ng/ml) and 0.16 μg/ml (160 ng/ml) injected and Rt. for NDMA 5.634 and NDEA 6.516 min, respectively. A linear/range lies in between 0.024 and 0.120 μg/ml and 0.048 and 0.240 μg/ml for NDMA and NDEA with r2 >0.99. The precision, accuracy, and system suitability are established as per USFDA and ICH guidelines, the sensitivity of NDMA limit of detection and limit of quantification 0.08, 0.024 and NDEA 0.16, 0.048. Conclusion: Other nitrosamine impurities are not involved in the determination of NDMA and NDEA in the OLM using GC-MS/MS and the method is simple, sensitive, rapid, accurate, and precise.

scholarly journals Quantitative determination and validation of ethylhexylglycerin using Gas chromatography method

2018 ◽  
Vol 9 (1) ◽  
pp. 30
Author(s):  
Rambabu Arla ◽  
Srinivasa Rao J ◽  
Kailasam Koumaravelou
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Stability Studies ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Clear Peak ◽  
Gas Chromatographic Method

Ethylhexylglycerin, an alkyl glyceryl ether, used in various cosmetics and deodorants is also known to have anti-microbial activity and hence used as an adjuvant along with other preservatives to produce synergistic effect. In the present study, a gas chromatographic method has been employed and validated to determine the presence of impurities along with ethylhexylglycerin. A column having the dimension of DB-1 30m x 0.32mm; 0.25µm with acetone as solvent was found to be optimal for the ideal separation of ethylhexylglycerin from its impurities. Injection volume was set to 1 µl and temperature was maintained at 240°C. A clear peak was observed with the retention time of 8.002 minutes. As per ICH guidelines, the developed method was validated with respect to specificity, sensitivity, Limit of detection, Limit of quantification, linearity, precision, and also stability studies. As per the method, it shows a good correlation co-efficient (R2) value of 0.999 within the concentration range of 0.1- 0.75µg. Therefore, a gas chromatographic method was proposed which can be precise, specific and can be employed for the determination of ethylhexylglycerin in various pharmaceutical formulations. Keywords: Ethylhexylglycerin; Adjuvant; ICH guidelines; Validation; Stability studies

Development and Validation of a Headspace Gas Chromatographic Method for the Determination of Methyl Bromide Content in Itraconazole API

2015 ◽  
Vol 59 ◽  
pp. 160-169
Author(s):  
Mannem Durga Babu ◽  
Medikondu Kishore ◽  
K. Surendra Babu
Keyword(s):  
Methyl Bromide ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Limit Of Quantitation ◽  
Headspace Gas ◽  
Current Article ◽  
Bulk Drug ◽  
Gas Chromatographic Method ◽  
Development And Validation

To provide quality control over the manufacture of any API, it is essential to develop highly selective analytical methods. Gas chromatography with headspace (HSGC) is widely used for the determination of residual impurities and solvents in API’s. In the current article we are reporting the development and validation of a rapid and specific Head space gas chromatographic (HSGC) method for the determination of methyl bromide in Itraconazole API. The developed method was validated in terms of specificity, linearity, precision, accuracy, limit of detection (LOD) and limit of quantitation (LOQ). The developed method was utilized for the investigation of methyl bromide content in bulk drug.

scholarly journals Detection and Quantitative Estimation of Toxic Acrylamide Levels in Selected Potatoes Chips and French Fries from the Libyan Market Using HPLC-UV Method

2021 ◽  
Vol 36 (2) ◽  
pp. 106-115
Author(s):  
Osama I. G. Khreit ◽  
Abdulsalam Elfowiris ◽  
Abdulrahman A. Aljali ◽  
Omukalthum Abduljalil
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Quantitative Estimation ◽  
Reversed Phase ◽  
French Fries ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Potential Health

Acrylamide is a potential health hazardous compound occurring in baked and fried food as a result of excessive dry heating during the preparation and/or processing of foods. Exposure to a high level of acrylamide may cause cancer, neurotoxicity, and mutagenicity. In this study, an isocratic reversed-phase high-performance liquid chromatographic (HPLC) method using a C18 column was used for the determination of acrylamide in selected food. The mobile phase consisted of 0.1% formic acid in water: acetonitrile (98:02), and the flow rate was 1.0 mL min-1, elution was monitored at 200 nm. Validation in selected conditions showed that the chosen method is sensitive, selective, precise, and reproducible with a linear detector response for the determination of acrylamide. The limit of detection (LOD), and the limit of quantification (LOQ), were achieved at 0.41μg mL-1 and 1.25 μg mL-1respectively. The proposed method was also applied after validation to the most popular six brands of chips and French fries available in the Libyan market. Acrylamide was extracted by a simplified extraction method avoiding cleanup by solid-phase extraction (SPE), then analyzed by HPLC-UV. The highest level of acrylamide was found in one brand of chips with a concentration of 16.33 μg mL-1, whereas only one of the French fries products analyzed exhibited an acrylamide concentration of 10.26 μg mL-1.

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