scholarly journals In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection

2017 ◽  
Vol 38 (6) ◽  
pp. 3539 ◽  
Author(s):  
Carolina Kato Prado ◽  
Flavio Dias Ferreira ◽  
Erika Bando ◽  
Miguel Machinski Junior

The indiscriminate use of antibiotics in dairy cattle without complying with the waiting period results in residual contamination, whose effective control in produced milk requires validated methods toensure analytical results. The aim of this study was to optimize and validate the HPLC-UV/VIS method at 365 nm for analyzingthe tetracycline in pasteurized cow milk in accordance with the European Community (2002/657/EC). Spiked milk with analytes (oxytetracycline, tetracycline, doxycycline, and chlortetracycline) was submitted to deproteinization and cleaning by a C18 solid-phase column and analyzed by HPLC using a gradient system with 0.01 mol L?1 oxalic acid-acetonitrile-triethylamine (90:9.9:0.1) and acetonitrile on a reverse phase (C18) column. Accuracy and precision were assessed by adding analytes to levels of 0.5, 1, and 1.5 times the permissible maximum limit allowed in Brazil. The method presented selectivity with a decision limit (CC?) and detection capability (CC?) ranging from 114.2 to 143.7 and from 129.3 to 188.7 µg kg?1, respectively. The recovery of tetracyclines was higher than 82.5% with a precision of 7.1%, demonstrating theefficiency in determining tetracycline residues in cow milk.

2013 ◽  
Vol 781-784 ◽  
pp. 99-103 ◽  
Author(s):  
Ling Lin ◽  
Chun Liang Yang ◽  
Zheng Peng ◽  
Ming Yue Wang ◽  
Zong Qiang Zeng ◽  
...  

A method was developed for simultaneous determination of imidacloprid,acetamiprid, thiabendazole and carbendazim in lentinus edodes, straw mushroom and oyster mushroom by HPLC. Acetonitrile was edded in the sample for extraction solvent, the sample was purified by NH2 solid phase extraction cartridge,then detected by HPLC.The results showed that a good linearity in the range of 0.05~5.0μg/mL with the linear correlation coefficients of 0.9991~0.9997, the detection limits of imidacloprid, acetamiprid, thiabendazole and carbendazim were respectively 0.002 mg/kg,0.005mg/kg, 0.003 mg/kg and 0.003 mg/kg.Tests for recovery were made by addition of four pesticidess standards at three different concentration levels (0.1, 0.5 and 1.0 mg/kg) to the blank sample.The mean recovery rates were 86.0%~105.0% , the relative standard deviations were less than 3.5%.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.


2021 ◽  
Vol 2 (3) ◽  
pp. 01-08
Author(s):  
Ali Jaber ◽  
Zeinab Zahreddine ◽  
Simon Abou Haidar ◽  
Chadi Hosri ◽  
Ghassan Ibrahim ◽  
...  

The existence of antibiotic residues in edible products constitutes a health problem to the consumers. Reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) was optimized and validated for the simultaneous determination of florfenicol (FF), penicillin (PE), and tetracycline (TC) residues in dairy raw milk samples. The determination of these antibiotics was carried out on HP-ODS Hypersil C18 (5μm, 125*4 mm) column at a flow rate (1mL/min) and temperature (35 ⁰C). The extraction method includes deproteinization of the milk sample followed by a solid-phase extraction (SPE) clean-up. The method was validated according to the European Commission Decision 2002/657/EC and the International Conference of Harmonization Guidelines. The recoveries for the studied antibiotics ranged from 82–111.54 % making the method suitable for performing routine analysis. The proposed method was applied for the analysis of antibiotic residues in 50 dairy raw milk samples collected from many regions in Lebanon. The results showed the occurrence of these antibiotics residues in milk collected from different Lebanese regions. The numbers indicate that 22 % of milk samples were found to be positive for FF, 42 % for PE, and 28 % for TC residues.


2012 ◽  
Vol 56 (4) ◽  
pp. 595-599 ◽  
Author(s):  
Teresa Szprengier-Juszkiewicz ◽  
Piotr Jedziniak ◽  
Małgorzata Olejnik ◽  
Jan Żmudzki

Abstract A sensitive and reliable method has been developed and validated to determine residues of abamectin, doramectin, eprinomectin, ivermectin, and moxidectin in bovine milk. Isolation of the analytes from milk was performed with the use of liquidliquid extraction with acetonitrile in the presence of sodium chloride. The extract was defatted with hexane and cleaned up using solid phase extraction (C8 cartridge) after forming ion pairs with triethylamine. The analytes were derivatized with N, Ndimethylformamide, acetic acid anhydride, and N-methylimidazole (100°C, 90 min). The derivatives were determined by reverse phase liquid chromatography with fluorescence detection (excitation and emission wavelength 365 nm and 475 nm, respectively). Recoveries of the lactones from milk samples fortified at 10-30 μg kg-1 ranged from 52% to 80% with intra-laboratory reproducibility (CV) of 12.7%-22.8%. The critical concentrations (decision limit, CCα and detection capability, CCβ) were in accordance with target limits. The method has been verified in the proficiency studies by EURL/CVL Berlin (all z-scores in the range of ±2). The method was transferred to routine laboratories, verified in inter-laboratory comparison and successfully applied in the National Residue Control Plan.


2014 ◽  
Vol 1004-1005 ◽  
pp. 914-918 ◽  
Author(s):  
Ling Lin ◽  
Hong Bin Guo ◽  
Qi Li ◽  
Li Qiang Zhang ◽  
Li Li Liu ◽  
...  

A sensitive method for simultaneously determining residues of oxytetracycline, tetracycline ,chlortetracycline and doxycycline in aquatic product was established by HPLC. Samples were extracted with Na2EDTA-Mcllvaine buffer solutions and centrifuged.The sample extracts were cleaned up by C18 solid-phase extraction cartridge and then were determined by UV detection at 355 nm.At fortification levels of 0.005~0.1 mg/kg, the average recoveries were of 75%~96% , The RSDs were of 1.02%~6.56%,Limit of detection was 0.002 mg /kg for oxytetracycline,tetracycline and doxycycline and 0.005 mg /kg for chlortetracycline.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.


Author(s):  
Bappa Ghosh ◽  
Arijita Bhattacharyya ◽  
Sandip Hingmire ◽  
Pushpa Aher ◽  
Pradnya Zende ◽  
...  

Abstract Background For years, turmeric has been used in several cuisines worldwide because of its proven health benefits. However, as its cultivation often involves applications of polar and semi-polar pesticides, their residues might cause health hazards to consumers. The dearth of a validated LC-MS/MS method for the residue analysis of these pesticides in turmeric has warranted the present study. Objective The aim was to develop and validate a multi-residue method for simultaneous determination of multi-class pesticides in turmeric (both rhizome and powder) by LC-MS/MS. Method Both the rhizome and powder samples (1 kg) were soaked in water for 30 min, followed by homogenization. Each homogenate (2 g) was mixed with 10 mL water, and extracted with acetonitrile (10 mL) in the presence of acetic acid and NaCl. The extract was cleaned by using dispersive solid phase extraction (dSPE) with graphitized carbon (5 mg/mL) sorbent. The cleaned extract was measured by LC-MS/MS with a runtime of 20 min. The method was validated on 211 multi-class pesticides. Results The method performance was satisfactory at 10 ng/g and higher levels, in compliance with the SANTE/12682/2019 guidelines. The dSPE cleanup was effective in minimizing the matrix effects. The use of matrix-matched calibrations specific for turmeric powder and rhizome corrected all recoveries within the satisfactory range of 70–120%. The precision -RSDs were <20% for all test pesticides. The Horwitz ratio and measurement uncertainty results were satisfactory as well. Conclusions As the method was convenient, selective, accurate, and repeatable, it is recommended for regulatory and commercial testing purposes. Highlights For the first time, this study reports a validated LC-MS/MS method for the multi-residue analysis of pesticides in turmeric. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision. The method performance satisfied the requirements of the SANTE/12682/2019 guidelines, and the method sensitivity complied with the EU-MRL requirements.


2009 ◽  
Vol 92 (2) ◽  
pp. 612-621 ◽  
Author(s):  
Hanwen Sun ◽  
Fengchi Wang ◽  
Lianfeng Ai ◽  
Chunhai Guo ◽  
Ruichun Chen

Abstract A sensitive method based on solid-phase extraction-liquid chromatography-tandem mass spectrometry interfaced with electrospray ionization (SPE-LC-MS/MS-ESI) was developed for the simultaneous determination of 8 banned nitroimidazole (NOZ) drugs including metronidazole (MNZ), ronidazole (RNZ), dimetridazole (DMZ), tinidazole, ornidazole, secnidazole, metronidazole-OH (MNZOH, the metabolite of MNZ), and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI, the metabolite of RNZ and DMZ) in natural casings. After extraction with ethyl acetate and evaporation, the NOZs were reconstituted in ethyl acetate and purified on a strong cation-exchange SPE column, and then LC/MS/MS analysis was performed by positive ESI applying multiple reaction monitoring of 2 transition reactions for each compound. The method was validated according to the European Union requirements (Commission Decision 2002/657/EC). Specificity, linearity, decision limit (CC), detection capability (CC), accuracy, and precision were determined. Average recoveries of the 8 NOZs from natural animal casing fortified at 3 levels (0.1, 0.5, and 1 g/kg) ranged from 87.3 to 116.5. The calculated CC for NOZs ranged from 0.029 to 0.049 g/kg, and CC ranged from 0.049 to 0.083 g/kg. Repeatability was in the range of 3.3510.1, and within-laboratory reproducibility was <10.3.


2013 ◽  
Vol 781-784 ◽  
pp. 1392-1396 ◽  
Author(s):  
Ling Lin ◽  
Zheng Peng ◽  
Chun Liang Yang ◽  
Ming Yue Wang ◽  
Yu Bing Zha ◽  
...  

The aim of this work was to establish a method that the residues of imidacloprid,carben-dazim and thiabendazole in fruits and vegetables were determined by HPLC.Acetonitrile was edded in the sample for extraction solvent, and using sodium chloride for absorbing water of the sample,then purified by NH2 solid phase extraction cartridge, the sample was detected by HPLC.Under the selected conditions,the detection limits of imidacloprid, carbendazim, thiabendazole were 0.002 mg/kg,0.003 mg/kg and 0.003 mg/kg respectively.Tests for recovery were made by addition of three pesticidess standards at three different concentration levels (0.1, 0.5 and 1.0 mg/kg) to the blank sample.The mean recovery rates of imidacloprid, carbendazimand thiabendazole were87.0%~99.2%,82.0%~96.0% and 80.0%~95.0% respectively , and the relative standard deviations were 0.52%~6.80%.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.


2020 ◽  
Vol 103 (6) ◽  
pp. 1498-1511 ◽  
Author(s):  
Bappa Ghosh ◽  
Narayan Kamble ◽  
Arijita Bhattacharyya ◽  
Chandrasekar Kandaswamy ◽  
Kaushik Banerjee

Abstract Background and objectives Turmeric is widely used as an ingredient of food and medicinal products. There exists no validated method for multi-residue analysis of pesticides in turmeric. Objective This study was undertaken to develop a simple and robust method for the quantitative determination of multi-class pesticides in turmeric powder and rhizome by GC-MS/MS. Method Initially, the samples were soaked in water for 30 min and homogenized to a fine paste. A portion of this paste (2 g) was extracted with acetonitrile (2 mL) and partitioned with hexane (2 mL) after adding 5 mL of 20% NaCl. The cleanup step involved dispersive solid phase extraction with graphitized carbon black (GCB, 5 mg/mL). Its performance was evaluated against primary secondary amine (PSA) and C18 sorbents. The cleaned extract was evaporated to dryness and reconstituted in ethyl acetate before GC-MS/MS analysis. The method was validated for a mixture of 208 multi-class pesticides at 10 ng/g and higher levels (i.e., 20 and 50 ng/g). Results The findings, which demonstrated a satisfactory recovery and precision (RSDs <20%) for all compounds at 10 ng/g and higher spiking levels, are aligned with the analytical quality control criteria of SANTE/12682/2019 guidelines. The cleanup effect of GCB was much superior to that of PSA, C18, and their combinations. The solvent exchange step with hexane was effective in removing co-extractives and minimizing matrix effects. Conclusions This method complies with the regulatory requirements and is fit-for-purpose for pesticide residue monitoring in turmeric. Highlights The study reports a validated GC-MS/MS method for multi-residue analysis of pesticides in turmeric for the first time. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision.


2020 ◽  
Vol 16 (7) ◽  
pp. 942-949
Author(s):  
Lekweiri Haiba Legrae ◽  
Mohamed Fadel Deida ◽  
Bah Mohamed Lemine Abdellahi ◽  
Mohamed Brahim Elkory ◽  
Ibrahima Ndiaye ◽  
...  

Background: This study reports an easy method of a veterinary drug investigation in raw milk, based on QuECHERS extraction followed by RP-HPLC-UV analysis. Use of this benchtop system was motivated by its availability and moderate cost relatively to other sophisticated methods such as LC-MS which are more efficient. Methods: This developed method has been optimized and then after validation according to EU legislation, it demonstrated good linearity with R²>0.997, acceptable peak resolution within a short time (<9.5 min) and good recovery of the analyzed drugs (OXY, ALZ and IVR, respectively 87.08, 99.02 and 92.01 %). Additionally, we applied the method to the analysis of cow milk, collected in Nouakchott, capital of Mauritania. Results: The obtained results indicated a mixed level of drug use according to targeted molecules. In 42% of sampled farms, the anti-parasitics IVR and ALZ were detected whereas the antibiotic OXY was detected in 50%. Conclusion: This investigation shows that 17% of the sampled farms exceeded European standards for IVR drug.


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