Determination of Imidacloprid, Carbendazim and Thiabendazole Residues in Vegetables and Fruits by HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 1392-1396 ◽  
Author(s):  
Ling Lin ◽  
Zheng Peng ◽  
Chun Liang Yang ◽  
Ming Yue Wang ◽  
Yu Bing Zha ◽  
...  
Keyword(s):  
Fruits And Vegetables ◽  
Solid Phase ◽  
Residue Analysis ◽  
Extraction Solvent ◽  
Solid Phase Extraction Cartridge ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Vegetables And Fruits ◽  
Concentration Levels

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.

Determination of Imidacloprid, Acetamiprid, Thiabendazole and Carbendazim Residues in Edible Fungi by HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 99-103 ◽  
Author(s):  
Ling Lin ◽  
Chun Liang Yang ◽  
Zheng Peng ◽  
Ming Yue Wang ◽  
Zong Qiang Zeng ◽  
...  
Keyword(s):  
Solid Phase ◽  
Residue Analysis ◽  
Correlation Coefficients ◽  
Edible Fungi ◽  
Extraction Solvent ◽  
Solid Phase Extraction Cartridge ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Straw Mushroom

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.

Determination of Tetracyclines Residues in Aquatic Products by HPLC

2014 ◽  
Vol 1004-1005 ◽  
pp. 914-918 ◽  
Author(s):  
Ling Lin ◽  
Hong Bin Guo ◽  
Qi Li ◽  
Li Qiang Zhang ◽  
Li Li Liu ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Residue Analysis ◽  
Pesticide Residue Analysis ◽  
Aquatic Products ◽  
Buffer Solutions ◽  
Aquatic Product ◽  
Solid Phase Extraction Cartridge ◽  
Accuracy And Precision

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.

Multiresidue Determination of Avermectins in Plant-Derived Food by UPLC-MS/MS

2012 ◽  
Vol 554-556 ◽  
pp. 1322-1326
Author(s):  
Yu Bing Zha ◽  
Chun Liang Yang ◽  
Ming Yue Wang ◽  
Yong Zhou Wang ◽  
Cheng Yu Luo ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Residue Analysis ◽  
Food Plant ◽  
Tandem Mass ◽  
Pesticide Residue Analysis ◽  
Accuracy And Precision ◽  
Multiresidue Determination ◽  
Concentration Levels

The objective of this study was to propose a method that the residues of avermectins (Abamectin, Emamectin Benzoate, Ivermectin, Eprinomectin and Doramectin) derived from the food plant were determined by UPLC-MS/MS. The avermectins were extracted with acetonitrile, purified by Alumina B or GCB/NH2 SPE cartridge, and then determined by ultra high-performance liquid chromatography with tandem mass spectrometry. Tests for recovery (Recovery rate: 80.6%～99.8%, RSD's: 0.22%～6.4%) were made by addition of avermectin standards at three different concentration levels (4, 20 and 100μg/kg) to five kinds of food plant as matrixes. The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.

scholarly journals Determination of Tylosin in Feeds by Liquid Chromatography with Solid-Phase Extraction

2004 ◽  
Vol 87 (2) ◽  
pp. 341-345 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson ◽  
James C Selkirk
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reversed Phase ◽  
Phase Extraction ◽  
Column Temperature ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard ◽  
Phase Liquid

Abstract A method was developed for the determination of tylosin in feeds. The method involves extraction of tylosin with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex C18 solid-phase extraction cartridge. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 285 nm with a reference wavelength of 320 nm with column temperature of 45°C. Average spike recoveries for samples prepared at 4 spiking levels (22.7, 181, 907, and 1000 g/ton) were 111.0, 94.9, 96.2, and 98.6%, respectively. The overall method precision at each of the 4 spiking levels was ≤ 7.85% relative standard deviation. The limits of detection and quantitation (g/ton) were 2.16 and 7.20 g/ton, respectively.

scholarly journals Determination of Six Pesticides in the Medicinal Herb Cordia salicifolia by Matrix Solid-Phase Dispersion and Gas Chromatography/Mass Spectrometry

2009 ◽  
Vol 92 (4) ◽  
pp. 1184-1189 ◽  
Author(s):  
Pedro Henrique Viana De Carvalho ◽  
Vanessa De Menezes Prata ◽  
Pricles Barreto Alves ◽  
Sandro Navickiene
Keyword(s):  
Extraction Method ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Neutral Alumina ◽  
Appetite Suppressant ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Concentration Levels

Abstract A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selectedion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexanedichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9, with relative standard deviations between 6.3 and 26. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.

scholarly journals Determination of Organophosphorus Pesticide Residues in the Roots of Platycodon grandiflorum by Solid-Phase Extraction and Gas Chromatography with Flame Photometric Detection

2006 ◽  
Vol 89 (1) ◽  
pp. 225-231 ◽  
Author(s):  
Xionghai Yi ◽  
Qing Hua ◽  
Yitong Lu
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Organophosphorus Pesticide ◽  
Phase Extraction ◽  
Platycodon Grandiflorum ◽  
Photometric Detection ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Flame Photometric Detection

Abstract Asimple and rapid sample preparation method using accelerated solvent extraction and solid-phase extraction (SPE) cleanup for determining organophosphorus (OP) pesticides in the roots of Platycodon grandiflorum was developed. The OP pesticides were concentrated by use of an SPE cartridge (ENVI-Carb) and quantitatively analyzed and confirmed by capillary gas chromatographywith flame photometric detection. The pesticides were eluted from the cartridges with 20mL acetonitriletoluene (3 1, v/v). The averag recovery from 10 g P. grandiflorum roots, fortified at 3 levels ranging from 0.04 to 1.00 mg/kg, was 91.9 with a relative standard deviation of 4.3. The limits of detection ranged from 1.16 103 mg/kg (dimethoate) to 4.64 103 mg/kg (dichlorvos). The proposed method showed acceptable accuracy and precision while minimizing environmental concerns, time, and labor.

scholarly journals Determination of Penicillin G in Feeds by Liquid Chromatography with Solid-Phase Extraction

2005 ◽  
Vol 88 (3) ◽  
pp. 679-683 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reversed Phase ◽  
Penicillin G ◽  
Phase Extraction ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method was developed for the determination of penicillin G in feeds. The method involves extraction of penicillin G with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex Strata-X solid-phase extraction cartridge. Analyte separation and quantification were achieved by gradient reversed-phase liquid chromatography and ultraviolet absorbance at 230 nm. Average spike recoveries for samples prepared at 3 spiking levels (25, 50, and 200 g/ton) were 96.3, 92.1, and 88.6%, respectively. The overall method precision at each of the 3 spiking levels was ≤5.39% relative standard deviation. The limits of detection and quantititation (g/ton formulation) were 3.89 and 13.0 g/ton, respectively.

scholarly journals Analysis and Evaluation of 7 Indictor Polychlorinated Biphenyls (PCBs) Residues in Dried Kelp by Gas Chromatography (GC)

2020 ◽  
Vol 165 ◽  
pp. 03044
Author(s):  
Liangliang Tian ◽  
Yongfu Shi ◽  
Dongmei Huang ◽  
Huijuan Yu ◽  
Shuai Wang ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Phase Extraction ◽  
Internal Standard Method ◽  
Neutral Alumina ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard

In this study, a special method was developed for the determination of 7 kinds of polychlorinated biphenyls (PCBs) residues in dried kelp by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/dichloromethane (1/1, v/v) by ultrasonic extraction. Clean-up methods were used by concentrated sulphuric acid, neutral alumina oxide solid phase extraction cartridge and silica solid phase extraction cartridge. The analytical compounds were quantified by an internal standard method. Under optimal experimental conditions, good linearity was observed in the range of 5~200ng/mL, and the correlation coefficients were 0.9993~0.9998. The limit of quantification (LOQ) for target analytical compounds ranged from 6.0 to 7.5μg/kg. At the spiked levels of 10，20，50 μg/kg，the average recoveries ranged from 81.8% to 105% with the relative standard deviations 3.05%～11.2%. The result showed that the proposed method was accurate and could be used for the determination of the PCBs in dried kelp.

scholarly journals Determination of Florfenicol in Fish Feed by Liquid Chromatography

2005 ◽  
Vol 88 (6) ◽  
pp. 1777-1783 ◽  
Author(s):  
John M Hayes
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase ◽  
Reversed Phase ◽  
Fish Feed ◽  
Water Mixture ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard ◽  
External Standard ◽  
Phase Liquid

Abstract A simple, accurate, and reproducible assay was developed for the determination of Florfenicol in medicated fish feed. Florfenicol was extracted from ground feed into an acetonitrile–water mixture by shaking and sonication. A portion of the centrifuged extract was passed through an Envi-Carb™ solid-phase extraction cartridge, through which Florfenicol eluted unretained. The collected eluant was diluted to adjust for analyte concentration, and injected into a reversed-phase liquid chromatography system. Samples were quantitated by external standard analysis versus multilevel calibration solutions. The procedure is suitable for the quantitation of samples medicated with 0.2–4 g/kg Florfenicol. Accuracy was evaluated by 2 analysts, who determined recovery of Florfenicol from feeds fortified over a range of 0.1–6.0 g/kg. The average recovery was 100.5% (relative standard deviation, 1.2%). The linearity, accuracy, precision, reproducibility (interday and analyst), and selectivity of the method are presented. The detection and quantitation limits were determined to be 0.2 and 1.0 mg/kg, respectively.

Simultaneous Determination of Aminopyralid, Clopyralid, and Picloram Residues in Vegetables and Fruits Using Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry

2012 ◽  
Vol 95 (2) ◽  
pp. 554-559 ◽  
Author(s):  
Yingying Tian ◽  
Xingang Liu ◽  
Fengshou Dong ◽  
Jun Xu ◽  
Caihong Lu ◽  
...  
Keyword(s):  
Residue Analysis ◽  
Ultra Performance Liquid Chromatography ◽  
The European Union ◽  
Analysis Method ◽  
Chromatography Tandem Mass Spectrometry ◽  
Maximum Residue Limits ◽  
Liquid Chromatography Tandem Mass ◽  
Vegetables And Fruits ◽  
Concentration Levels

Abstract A sensitive and effective method for the simultaneous quantitative determination of aminopyralid, clopyralid, and picloram in vegetables (eggplant, cucumber, and tomato) and fruits (apple and grape) was developed and validated using ultra-performance LC coupled with MS/MS. The three herbicides were successfully separated and independently confirmed in a single run. Different extraction and cleanup methods were used to optimize the pretreatment processes of the residue analysis method. The final method is straightforward and involves extraction with 1% formic acid–acetonitrile, and no complicated cleanup process is needed. Determination of the compounds was achieved within 3.0 min. Respective average recoveries using this method at four concentration levels (0.05, 0.1, 0.5, and 1.0 mg/kg) ranged from 66.5 to 109.4%, with RSDs in the range of 1.1–19.7% (n = 5) for all analytes. The LODs were below 0.010 mg/kg, and the LOQs did not exceed 0.036 mg/kg, which were lower than the maximum residue limits (MRLs) of 0.5–5.0 mg/kg clopyralid in vegetables and fruits samples, as established by the European Union. This study provides a theoretical basis for China to develop MRLs and an analytical method for aminopyralid, clopyralid, and picloram in vegetables and fruits.

Sign in / Sign up

Export Citation Format

Share Document