scholarly journals ELISA validation and determination of cut-off level for chloramphenicol residues in honey

2015 ◽  
Vol 59 (3) ◽  
pp. 353-356 ◽  
Author(s):  
Bogumił Biernacki
Keyword(s):  
Matrix Effects ◽  
Screening Methods ◽  
Analytical Validation ◽  
Detection Capability ◽  
Elisa Method ◽  
Related Substances ◽  
Veterinary Medicines ◽  
Acetate Mixture ◽  
Ethyl Acetate Mixture

Abstract An analytical validation of a screening ELISA for detection of chloramphenicol (CAP) in honey was conducted according to the Commission Decision 2002/657/EC and Guidelines for the Validation of Screening Methods for Residues of Veterinary Medicines. The analyte was extracted from honey with a water and ethyl acetate mixture, and CAP concentrations were measured photometrically at 450 nm. The recovery rate of the analyte from spiked samples was 79%. The cut-off level of CAP in honey as the minimum recovery (0.17 units) was established. Detection capability (CCβ) was fixed at 0.25 μg kg−1. No relevant interferences between matrix effects and structurally related substances including florfenicol and thiamphenicol were observed. The ELISA method should be useful for determination of CAP residues in honey monitoring.

scholarly journals ELISA validation and determination of cut-off level for chloramphenicol (CAP) residues in shrimp and fish

Our Nature ◽  
2017 ◽  
Vol 15 (1-2) ◽  
pp. 13-18 ◽  
Author(s):  
Md. Golam Sarwer ◽  
Md. Mahmudul Hasan Rony ◽  
MSt. S. Sharmin ◽  
A.K. Jilani Chowdhury ◽  
Shuva Bhowmik
Keyword(s):  
Matrix Effects ◽  
Enzyme Linked Immunosorbent Assay ◽  
Screening Methods ◽  
Analytical Validation ◽  
Detection Capability ◽  
Related Substances ◽  
Veterinary Medicines ◽  
Acetate Mixture ◽  
Ethyl Acetate Mixture

An analytical validation of enzyme-linked immunosorbent assay (ELISA) screening for detection of chloramphenicol (CAP) in shrimp and fish was conducted according to the Commission Decision 2002/657/EC and guidelines for the validation of screening methods for residues of veterinary medicines. The analyte was extracted from shrimp and fish with ethyl acetate mixture, and CAP concentrations were measured photometrically at 450 nm. The recovery rate of the analyte from spiked samples was 80%. For the laboratory the cut-off level of CAP in fish and shrimp as the minimum recovery was established along with detection capability (CCβ). No relevant interferences between matrix effects and structurally related substances including florfenicol and thiamphenicol were observed. The experimental results were quite satisfactory and ELISA method was found very useful for determination of CAP residues in shrimp and fish monitoring.

scholarly journals Валідація методу кількісного визначення нітрофурану (АОЗ) і хлорамфеніколу у зразках меду натурального за допомогою тест-системи RidaScreen®

2018 ◽  
Vol 8 (1) ◽  
pp. 892-897
Author(s):  
K.S. Myagka ◽  
S.A. Tkachuk ◽  
N.A. Mezhenska
Keyword(s):  
Screening Method ◽  
Test System ◽  
Screening Methods ◽  
Detection Capability ◽  
Initial Validation ◽  
Veterinary Medicines ◽  
Allowable Level ◽  
Validation Parameters ◽  
Natural Honey

<p><span lang="EN-US">We presented the validation method of the quantitative determination of Nitrofuran (AOZ) and Chloramphenicol in honey samples by the RidaScreen® test system (according to Commission Decision 2002/657/EC and Guidelines for the validation of screening methods for residues of veterinary medicines (initial validation and transfer) of 20/01/2010). We revealed several validation indicators like ccβ (detection capability), accuracy (precision), recovery and some others during the initial validation (specificity and selectivity). We determined the minimum detection values of Nitrofuran (AOZ) in honey, the highest value (the highest response) for blank samples is 0.066 μg/kg and the lowest value for enriched samples (lowest response) is 0.401 μg/kg. Based on the obtained results none of the responses for enriched samples do not coincide with the range of replies of blank samples. Hence, it follows that the detection capability (CCβ) for this screening method is less than or equal to 0.4 μg/kg. For the determination of Chloramphenicol, the highest response is noted for blank samples – 0.021 μg/kg (21 ng/kg) and the lowest response noted for enriched samples is 0.048 μg/kg (48 ng/kg). None of the responses for enriched samples do not coincide with the range of replies of blank matrix (samples), therefore we could conclude that the CCβ of this screening method is less than or equal to 0.05 μg/kg (β-error &lt; 5 %) and the cut-off value of this test is 0.048. According to the validation the lowest value of substances that could detected by ELISA using the following test systems for competitive ELISA (enzyme-linked immunoassay) for Nitrofuran (AOZ) – 0.4 μg/kg, for Chloramphenicol </span><span lang="UK">–</span><span lang="EN-US"> 0.05 μg/kg. Described in State Standard 4497:2005 “Natural Honey. Technical conditions” the maximum allowable level for Chloramphenicol </span><span lang="UK">–</span><span lang="EN-US"> 0.3 μg/kg and Nitrofuran (AOZ) </span><span lang="UK">–</span><span lang="EN-US"> 0.6 μg/kg require</span><span lang="EN-US">correction according to the established validation parameters. </span></p>

scholarly journals A New Lc-Ms/Ms Method for Multiple Residues/Contaminants In Bovine Meat

2020 ◽  
Author(s):  
Zehra Hajrulai-Musliu ◽  
Risto Uzunov ◽  
Stefan Jovanov ◽  
Dean Jankuloski ◽  
Velimir Stojkovski ◽  
...  
Keyword(s):  
Coefficient Of Variation ◽  
Matrix Effects ◽  
Limit Of Detection ◽  
Veterinary Drug ◽  
Detection Capability ◽  
Limit Of Quantification ◽  
Internal Standards ◽  
Anabolic Hormones ◽  
Residual Matrix

Abstract A multi-class and multi-residue/contaminant method for the determination of veterinary drug and pesticide residues and mycotoxins in bovine meat has been developed and validated. The veterinary drug residues/contaminants included antimicrobials, anabolic hormones, lactones, β-agonists, mycotoxins, and pesticides. Isotopic labeled internal standards were included to compensate residual matrix effects. The calibrators used in the method demonstrated linearity with the coefficient of correlation (R2) > 0.98. The decision limit (CCα) values were in the range from 0.067 to 2103.84 μg/kg, while the range for detection capability (CCβ) was from 0.083 to 2482.13 μg/kg. The limit of detection (LOD) and limit of quantification (LOQ) were in the range from 0.059 to 291.36 μg/kg, and 0.081 to 328.13 μg/kg, respectively. The recovery of analytes ranged from 61.28 % to 116.20 %. The intra-day coefficient of variation (CV) was from 0.97 to 25.93 % and the inter-day CV was 2.30-34.04 %. The method has been used for the determination of 49 residues/contaminants in bovine meat.

scholarly journals A new LC–MS/MS method for multiple residues/contaminants in bovine meat

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Zehra Hajrulai-Musliu ◽  
Risto Uzunov ◽  
Stefan Jovanov ◽  
Dean Jankuloski ◽  
Velimir Stojkovski ◽  
...  
Keyword(s):  
Coefficient Of Variation ◽  
Matrix Effects ◽  
Limit Of Detection ◽  
Veterinary Drug ◽  
Detection Capability ◽  
Limit Of Quantification ◽  
Internal Standards ◽  
Anabolic Hormones ◽  
Residual Matrix

AbstractA multi-class and multi-residue/contaminant method for the determination of veterinary drug and pesticide residues and mycotoxins in bovine meat has been developed and validated. The veterinary drug residues/contaminants included antimicrobials, anabolic hormones, lactones, β-agonists, mycotoxins, and pesticides. Isotopic labeled internal standards were included to compensate residual matrix effects. The calibrators used in the method demonstrated linearity with the R2 > 0.98. The decision limit (CCα) values were in the range from 0.067 to 2103.84 μg/kg, while the range for detection capability (CCβ) was from 0.083 to 2482.13 μg/kg. The limit of detection (LOD) and limit of quantification (LOQ) were in the range from 0.059 to 291.36 μg/kg, and 0.081 to 328.13 μg/kg, respectively. The recovery of analytes ranged from 61.28% to 116.20%. The intra-day coefficient of variation (CV) was from 0.97 to 25.93% and the inter-day CV was 2.30–34.04%. The method has been used for the determination of 49 residues/contaminants in bovine meat. Application of the method in routine analysis in bovine samples, revealed in limited samples the presences of enrofloxacin, oxytetracycline and sulfadiazine at the concentration of 35.22 µg/kg, 27.35 µg/kg, and 36.20 µg/kg, respectively.

Simultaneous Determination of Methocarbamol and Paracetamol in the Presence of Three Related Substances by Ultra Performance Liquid Chromatography

2019 ◽  
Vol 15 (5) ◽  
pp. 505-510
Author(s):  
Yanjuan Zheng ◽  
Qiushi Peng ◽  
Rui Dong ◽  
Tingyu Chen ◽  
Yi Bao ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Pharmaceutical Preparations ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Related Substances ◽  
Bulk Powder ◽  
Highly Sensitive ◽  
Optimal Protocol ◽  
Acquity Uplc

Introduction: A rapid, and accurate Ultra Performance Liquid Chromatography (UPLC) method was developed to simultaneously analyze Methocarbamol, Paracetamol and the related substances Materials and Methods: Waters ACQUITY UPLC® BEH Phenyl C18 column was used in conjunction with UV detection at 225nm. Gradient elution with 0.05M, pH 6 phosphate buffer and acetonitrile flow at 0.3mL /min rate were used to separate the substances. The retention times for 4-Aminopheno, Paracetamol, Guaifenesin, Methocarbamol, and 4-Chloroacetanilide were 1.319 minute, 2.224 minute, 4.467 minute, 4.769 minute and 5.433 minute respectively. The concentration was linear in the range of 2-100 µg/ml for Methocarbamol, and 1-100 µg/mL for Paracetamol. The percentage recoveries were between 99.28±1.23% to 100.57±0.99% for Methocarbamol, and between 99.08±1.23% to 101.23±1.39% for Paracetamol. Results and Discussion: The validated optimal protocol is robust and accurate for simultaneous analysis of Methocarbamol, Paracetamol and the related substances, applicable for bulk powder as well as pharmaceutical formulation. Conclusion: In this paper, a highly sensitive, accurate, and precise UPLC method with UV-Vis detection was developed and validated for quality control of MET and PAR in bulk as well as in pharmaceutical preparations.

Determination of spectinomycin hydrochloride and its related substances by HPLC–ELSD and HPLC–MSn

2006 ◽  
Vol 834 (1-2) ◽  
pp. 178-182 ◽  
Author(s):  
Jian Wang ◽  
Xiaojun Hu ◽  
Ying Tu ◽  
Kunyi Ni
Keyword(s):  
Related Substances

scholarly journals Development of new spectrophotometric method for estimation of tenofovir disoproxil fumarate using MBTH reagent

2015 ◽  
Vol 4 (4) ◽  
pp. 378-381 ◽  
Author(s):  
Mannem Sri Varsha ◽  
N. Raghavendra Babu ◽  
Yenumula Padmavathi ◽  
P. Ravi Kumar
Keyword(s):  
Tenofovir Disoproxil Fumarate ◽  
Visible Region ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Journal ◽  
Specific Procedure ◽  
Analytical Validation ◽  
Pharmaceutical Dosage Forms ◽  
Secondary Amine Group ◽  
Validation Procedure

A new simple, sensitive and specific procedure has been developed for determination of tenofovir disoproxil fumarate in bulk and pharmaceutical dosage forms using MBTH reagent. The purpose of this analytical validation procedure is to validate it by laboratory experiments to prove that the method meets the minimum standards for laboratory use. 3-methyl-2-bezothiazoline hydrazone reacts with the secondary amine group of tenofovir in the presence of oxidizing agent, ferric chloride. The resulting apple green coloured chromogen when measured spectrophotometrically in visible region (i.e., 400-800nm) shows a maximum absorbance at 626.5nm. This method can be successfully applied for the determination of drug content in pharmaceutical formulations. The results of analysis have been validated statistically.DOI: http://dx.doi.org/10.3329/icpj.v4i4.22620 International Current Pharmaceutical Journal, March 2015, 4(4): 378-381 

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