scholarly journals Development and Validation of a Gas Chromatographic Method for the Quantification of Minor Alkaloids in Cocaine

2021 ◽  
Author(s):  
Adriano Maldaner ◽  
Jorge Zacca ◽  
Élvio Botelho ◽  
Dina Silva ◽  
Fillipe Oliveira
Keyword(s):  
Law Enforcement ◽  
Forensic Analysis ◽  
Thermal Processes ◽  
Flame Ionization ◽  
Target Analytes ◽  
Relative Standard ◽  
Parameter Variations ◽  
Analytical Parameter ◽  
Gas Chromatographic Method ◽  
Development And Validation

The quantification of minor alkaloids in seized cocaine can provide information for drug profiling and law enforcement initiatives. This work presents the development and validation of an analytical method to quantitate minor alkaloids in cocaine samples using gas chromatography with flame ionization detector, after derivatization. The method was validated in accordance with the ISO/IEC 17.025:2017 requirements. The calibration was linear (determination coefficient (R2) ≥ 0.998), ranging from 1.0 to 3,500 mg L-1 for all target analytes with suitable selectivity and precision (relative standard deviation lower than 10%). The method showed stability and robustness with respect to analytical parameter variations and presented good accuracy (recovery ranging from 90 to 108%). The method was considered adequate to routine forensic analysis in simultaneous quantification of anhydroecgonine methyl ester, anhydroecgonine, methylecgonine, tropacocaine, norcocaine, N-formylcocaine, trimethoxycocaine, ecgonine, benzoylecgonine, trans- and cis-cinnamoylcocaine. Eleven cocaine samples seized in different Brazilian regions were analyzed and their relative amounts of tropacocaine and trimethoxycocaine with respect to cocaine indicate both the possible varieties of coca leaf used for cocaine production and the likely origin of drug samples (Bolivia/Peru or Colombia). The contents of other minor alkaloids depict aspects of sample history such as purification by oxidation, hydrolysis and dehydration by thermal processes.

Gas Chromatographic Method for Quantitation and Confirmation of Trichothecenes in Wheat

1995 ◽  
Vol 78 (2) ◽  
pp. 386-390 ◽  
Author(s):  
Eliana B Furlong ◽  
Lucia M Valente Soares
Keyword(s):  
Chromatographic Method ◽  
Internal Standard ◽  
Chromatographic Behavior ◽  
Flame Ionization ◽  
Relative Standard ◽  
Group A ◽  
Standard Deviations ◽  
Group B ◽  
Gas Chromatographic Method ◽  
Derivatives Of

Abstract A capillary gas chromatographic method with flame ionization detection was evaluated for quantitation and confirmation of 7 trichothecenes known to occur in grain crops. The method was applied to spiked and naturally contaminated wheat samples. Samples were extracted with methanol-aqueous KCI. After clarification with ammonium sulfate and partition to chloroform, a charcoal–alumina–Celite column cleanup was used. Heptafluorobutyryl derivatives of trichothecenes were quantitated with a methyl eicosanoate internal standard. Confirmation of identity was achieved by comparing the chromatographic behavior of suspected samples with those of standards after acetylation and hydrolysis for group A trichothecenes, and acetylation and reduction for group B trichothecenes. Limits of detection ranged from 0.1 to 0.5 μg/g. Average recoveries for diacetoxyscirpenol (DAS) and nivalenol (NIV) determined at 7 levels of contamination were 88 and 93%, respectively. Average recoveries for deoxynivalenol, NIV, DAS, T2 tetraol, and T2 triol at a single level of contamination were 85,87,83,87, and 91 %, respectively. Relative standard deviations for determinations of naturally contaminated samples ranged from 2.8 to 12.9%. For spiked wheat samples, the relative standard deviations ranged from 4.6 to 11.9%.

Gas Chromatographic Method for Determination of p,p'-DDT in DDT Technical and Formulated Products: Collaborative Study

1990 ◽  
Vol 73 (5) ◽  
pp. 744-748
Author(s):  
Dwight L Mount ◽  
Frederick C Churchill
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Matched Pairs ◽  
Flame Ionization Detection ◽  
Flame Ionization ◽  
Paired Samples ◽  
Relative Standard ◽  
Gas Chromatographic Method ◽  
International Collaborative Study

Abstract A gas chromatographic (GC) method for determination of p,//-DDT In technical and formulated products was developed and It performed well in an initial small collaborative study among 4 laboratories. Samples are dissolved in chloroform, and p,p'-DDT is separated on an OV-210 column and determined by GC analysis with flame Ionization detection. 2,2'-Dlnltroblphenyl Is used as an Internal standard. The method was subjected to an International collaborative study with 10 participating laboratories. Collaborators received matched pairs of technical DDT products and of water-dlsperslble powder, emulslflable concentrate, and dustable powder formulations. Relative standard deviations for reproducibility (RSDR) for the paired samples were 1.16, 1.48, 2.08, and 1.80%, respectively. The method has been approved Interim official first action by AOAC as a CIPACAOAC method.

Development and Validation of Head-space Gas Chromatographic Method in Tandem with Flame ionized detection for the determination of Residual solvents in Simeprevir API Synthesis

2021 ◽  
pp. 5175-5181
Author(s):  
C. Hazarathaiah Yadav ◽  
A. Malli Babu
Keyword(s):  
Limit Of Detection ◽  
Intermediate Precision ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Flame Ionization ◽  
Limit Of Quantitation ◽  
Reference Material Certification ◽  
Precision System ◽  
Gas Chromatographic Method ◽  
Development And Validation

Residual solvent testing is an integral part of reference material certification. A gas chromatography/flame ionization detector/headspace method has been developed and validated to detect and quantitate commonly used residual solvents in our production processes: Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane in Simeprevir API. A simple and selective HS-GC method is described for the determination & quantification of Residual Solvents in Simeprevir API. Chromatographic separation was achieved on USP G43 equivalent capillary column Thermo Scientific™ Trace GOLD™ TG-624 SilMS, 30m × 0.32mm × 1.8µm column (P/N 26059-3390) using nitrogen as carrier gas by using different temperature gradient of FID Detectors. Linearity was observed in the range 40-120% of standard concentrations for Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane (r2>0.999) for the amount of solvent estimated by the proposed methods was in good agreement. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered diluent and API. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 10 for Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical active ingredients for estimation of Residual Solvents of Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane in Simeprevir. Baseline separation of all five solvents and Simeprevir API is achieved within 20.5 minutes of analysis time. Method validation comprised the following parameters: limit of detection (LOD), limit of quantitation (LOQ), linearity and range, accuracy, precision (repeatability and intermediate precision), system suitability, specificity, and robustness. Linearity and LOQ (ppm) are listed for each solvent in manuscript. The present method was proven to be robust and accurate for quantitative analysis of residual solvent in neat materials.

Simultaneous Determination of Chlorothalonil and Hexachlorobenzene in Technical and Formulated Materials by Capillary Gas Chromatography

1995 ◽  
Vol 78 (3) ◽  
pp. 604-609
Author(s):  
Linda D Vargyas ◽  
Gregory E Walls ◽  
Richard L Cryberg ◽  
William R Bramstedt ◽  
Frank J Wang ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Additional Method ◽  
Flame Ionization ◽  
Relative Standard ◽  
Technical Material ◽  
Solvent Systems ◽  
Butyl Phthalate ◽  
Gas Chromatographic Method ◽  
Influence Of Ph

Abstract A capillary gas chromatographic method using flame ionization detection was developed for simultaneous assay of chlorothalonil and hexachlorobenzene in technical material and formulated products. Method precision is excellent, and the method allows simultaneous determination of one chemical impurity. The method uses an internal normalization reagent (n-butyl phthalate). Modification and extension of the method to formulated products, including wettable powders, water-based flowables, and dispersible (or dry flowable) granular formulations, are discussed. Preliminary statistical analysis of intra- and interlaboratory comparisons was performed to evaluate method ruggedness. Average relative standard deviations for technical materials were 0.34 and 0.17% from 2 laboratories. Additional method validation studies were conducted to examine the influence of pH, solvent systems, gas chromatographic systems, and temperature conditions on different formulations.

scholarly journals Development and Validation of a UHPLC-qTOF MS Method for the Determination of Sorbitol-Based Nuclear Clarifying Agents in Food Simulants after Migration from Food Contact Materials

2021 ◽  
Vol 11 (9) ◽  
pp. 3789
Author(s):  
Emmanouil D. Tsochatzis ◽  
Georgios Theodoridis ◽  
Helen G. Gika
Keyword(s):  
A Posteriori ◽  
Contact Materials ◽  
Food Contact ◽  
Food Simulants ◽  
Target Analytes ◽  
Commission Regulation ◽  
Development And Validation ◽  
Migration Testing ◽  
Analytical Standards

Nuclear clarifying agents (NCAs) are a class of substances frequently used as additives in the production of polymers to improve their physical properties. Some are EU regulated under Commission Regulation (EU) no. 10/2011 can be used as additives in the production of food contact plastics. However, limited analytical methods for their analysis are currently available, in part due to poor solubility in most common organic solvents and lack of analytical standards of known purity. In this work, a simple and sensitive method was developed to analyze 4 EU-regulated sorbitol-based nucleating agents in food simulants, following solubility studies to establish effective solvents. The method was shown to be accurate and precise and can be used with official food simulant D1 (50% v/v ethanol/H2O). Application to other ethanolic simulants is also possible, but due to solubility issues, a posteriori conversion of those simulants into simulant D1 is required. Finally, the method was applied to quantify the target analytes in simulants after migration testing with polypropylene (PP) beverage cups.

Ayurvedic formulations containing benzoic and ascorbic acids as additives: benzene formation during storage and impact of additives on quality parameters

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Priyanka Sharma ◽  
Mukesh Maithani ◽  
Vikas Gupta ◽  
Parveen Bansal
Keyword(s):  
Ascorbic Acid ◽  
Quality Parameters ◽  
Over The Counter ◽  
Flame Ionization ◽  
Class 1 ◽  
Short And Long Term ◽  
Pharmaceutical Industries ◽  
Increasing Demand ◽  
Gas Chromatographic Method ◽  
Ascorbic Acids

AbstractObjectivesAyurvedic formulations are becoming the prior choice of people as health care supplements. The increasing demand for these formulations has led to extensive development of Ayurvedic pharmaceutical industries worldwide. The reaction between the preservatives (sodium benzoates and ascorbic acid) used in these formulations could generate benzene. Benzene is classified as class-1 human carcinogen and responsible for various short and long term health effects.MethodsIn this study, 25 formulations (containing ascorbic acid and sodium benzoate) of various manufacturers available as over the counter products were obtained and their benzene content were determined using gas chromatograph with flame ionization detector.ResultsThe result showed that 64% of the formulations were free from benzene contamination whereas 36% of formulations were found to be contaminated with benzene. A simple, less time-consuming, economic, and validated gas chromatographic method for estimation of benzene in Ayurvedic formulations was also developed successfully in present study.ConclusionsThe data revealed that the level of benzene was within permissible limits, yet the presence of a carcinogen in the marketed formulations intended for internal use is an alarming situation.

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 The Development and Validation of a Novel Designer Benzodiazepines Panel by LC–MS-MS

2021 ◽  
Author(s):  
Rebecca A Mastrovito ◽  
Donna M Papsun ◽  
Barry K Logan
Keyword(s):  
Illicit Drug ◽  
Liquid Extraction ◽  
Electrospray Tandem Mass Spectrometry ◽  
Method Performance ◽  
Internal Standards ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Development And Validation ◽  
Positive Ion ◽  
Designer Benzodiazepines

Abstract Novel illicit benzodiazepines are among the most active areas of new illicit drug manufacture and use. We describe a method for the detection and quantification of etizolam and its metabolite α-hydroxyetizolam, flubromazolam, clonazolam, diclazepam, delorazepam, bromazepam, flubromazepam, phenazepam, flualprazolam, flunitrazolam, and nitrazolam in human whole blood. After addition of internal standards, samples are buffered and extracted using a liquid–liquid extraction. Analysis is performed using positive-ion electrospray tandem mass spectrometry for detection and quantitation. Calibration ranges were established based on the method performance and differed from compound to compound. Replicates at the lowest calibration point for each compound performed within 5% of CV (Coefficient of Variation). The correlation coefficient was >0.990 for all compounds. Relative standard deviation for all compounds was ≤10% of CV and accuracy was  ±10% for both within- and between-run experiments. The maximum average intra- and inter-run imprecision were 5.7%. The maximum average intra- and inter-run imprecision was −8.7%. As part of evaluating the scope for relevancy, samples testing positive in immunoassay but confirmed to be negative in traditional benzodiazepine confirmation method were re-analyzed using this method. The presence of at least one novel benzodiazepine was identified in 70% of these samples. The appearance of these novel “designer” benzodiazepines demonstrates the challenge for toxicology testing and the need for continually updated confirmation methods.

Gas Chromatographic Method for Determination of Dimethylamine, Trimethylamine, and Trimethylamine Oxide in Fish-Meat Frankfurters

1991 ◽  
Vol 74 (2) ◽  
pp. 400-403
Author(s):  
Walter Fiddler ◽  
Robert C Doerr ◽  
Robert A Gates
Keyword(s):  
Atlantic Menhaden ◽  
Chromatographic Technique ◽  
Acid Extraction ◽  
Fish Meat ◽  
Flame Ionization ◽  
Trimethylamine Oxide ◽  
Headspace Gas ◽  
Gas Chromatographic Method ◽  
Gas Tight

Abstract A method Is described for analysis of minced fish-meat and surlmi-meat frankfurters for dimethylamine (DMA), trimethyiamine (TMA), and trimethyiamine oxide (TMAO) using a headspace-gas chromatographic technique. After simple acid extraction and addition of NaOH, the headspace was directly Injected Into a gas chromatograph by a gas-tight syringe. DMA and TMA were separated on a Chromosorb 103 column and detected by a flame Ionization detector. TMAO was measured as TMA after Zn reduction. Repeatability of the method for DMA, TMA, and TMAO was 6.6,1.0, and 18.8 ppm, respectively. The method was applicable to Alaska pollock-meat and Atlantic menhaden-meat frankfurters, unwashed, and washed mince and surlml.

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)  

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