scholarly journals Simultaneous Determination of Albendazole and Its Three Metabolites in Pig and Poultry Muscle by Ultrahigh-Performance Liquid Chromatography-Fluorescence Detection

Foods ◽  
2021 ◽  
Vol 10 (10) ◽  
pp. 2350
Author(s):  
Zhaoyuan He ◽  
Zhixiang Diao ◽  
Yawen Guo ◽  
Kaizhou Xie ◽  
Lan Chen ◽  
...  

A fast, simple and efficient ultrahigh-performance liquid chromatography-fluorescence detection (UPLC-FLD) method for the determination of residues of albendazole (ABZ) and its three metabolites, albendazole sulfone (ABZ-SO2), albendazole sulfoxide (ABZ-SO), and albendazole-2-aminosulfone (ABZ-2NH2-SO2), in pig and poultry muscle (chicken, duck and goose) was established. The samples were extracted with ethyl acetate, and the extracts were further subjected to cleanup by utilizing a series of liquid–liquid extraction (LLE) steps. Then, extracts were purified by OASIS® PRiME hydrophilic-lipophilic balance (HLB) solid-phase extraction (SPE) cartridges (60 mg/3 mL). The target compounds were separated on an ACQUITY UPLC® BEH C18 (2.1 mm × 100 mm, 1.7 μm) chromatographic column, using a mobile phase composed of 31% acetonitrile and 69% aqueous solution (containing 0.2% formic acid and 0.05% triethylamine). The limits of detection (LODs) and limits of quantification (LOQs) of the four target compounds in pig and poultry muscle were 0.2–3.8 µg/kg and 1.0–10.9 µg/kg, respectively. The recoveries were all above 80.37% when the muscle samples were spiked with the four target compounds at the LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL, and 2.0 MRL levels. The intraday relative standard deviations (RSDs) were less than 5.11%, and the interday RSDs were less than 6.29%.

2003 ◽  
Vol 86 (3) ◽  
pp. 612-622 ◽  
Author(s):  
Jitka Zrostlíková ◽  
Jana Hajšlová ◽  
Tomáš Kovalczuk ◽  
Radim Štěpán ◽  
Jan Poustka

Abstract A simple liquid chromatography/mass spectrome-try (LC/MS) approach for the determination of widely used representatives of polar/thermolabile pesticides in fruits was developed and validated. The group of pesticides comprised benzimidazoles and azoles (carbendazim, thiabendazole, imazalil, propiconazole, prochloraz, epoxiconazole, flusilazole, tebuconazole, bitertanol); N-methylcarbamates (carbaryl, carbofuran, methiocarb); and phenylureas and benzoylphenylureas (linuron, diflubenzuron, triflumuron, teflubenzuron, flufenoxuron). Matrixes (apple, apricot) were extracted with acetonitrile and crude extracts were cleaned up by solid-phase ex-traction (SPE) using either mixed cation exchange or hydrophilic lipophilic balance cartridges. LC separation of pesticides was performed on a reversed-phase column, Discovery C18. Electrospray ionization and ion trap MS/MS detection were applied. For most pesticides, overall recoveries ranged from 75 to 122%, and repeatability (as relative standard deviation) from 5 repetitive determinations of recovery ranged from 3 to 21%. Carbofuran was the only compound for which recovery was not satisfactory due to its loss in the SPE cleanup step. Limits of detection were 0.1–3 μg/kg for benzimidazole and azole fungicides and carbamate insecticides. For urea insecticides, detection limits were slightly higher (3–10 μg/kg).


1999 ◽  
Vol 82 (3) ◽  
pp. 614-619 ◽  
Author(s):  
Steven M Plakas ◽  
Kathleen R El Said ◽  
F Aladar Bencsath ◽  
Steven M Musser ◽  
Calvin C Walker

Abstract Rapid methods are described for determination of flumequine (FLU) residues in muscle and plasma of farm-raised channel catfish (Ictalurus punctatus). FLU residues were extracted from tissues with an acidified methanol solution, and extracts were cleaned up on C18 solid-phase extraction cartridges. FLU concentrations were determined by liquid chromatography (LC)using a C18 analytical column and fluorescence detection (excitation, 325 nm; emission, 360 nm). Mean recoveries of FLU from fortified muscle were 87–94% at 5 levels ranging from 10 to 160 ppb (5 replicates per level). FLU recoveries from fortified plasma were 92–97% at 5 levels ranging from 20 to 320 ppb. Limits of detection (signal-to-noise ratio, 3:1)for the method as described were 3 and 6 ppb for muscle and plasma, respectively. Relative standard deviations (RSDs) for recoveries were ≤12%. Live catfish were dosed with 14C-labeled or unlabeled FLU to generate incurred residues. Recoveries of 14C residues throughout extraction and cleanup were 90 and 94% for muscle and plasma, respectively. RSDs for incurred FLU at 2 levels in muscle and plasma ranged from 2 to 6%. The identity of FLU in incurred tissues was confirmed by LC/mass spectrometry.


2009 ◽  
Vol 59 (4) ◽  
pp. 805-813 ◽  
Author(s):  
L. Shi ◽  
X. F. Zhou ◽  
Y. L. Zhang ◽  
G. W. Gu

Fluoroquinolones (FQs) are among the most important antibiotics used in human and veterinary medicines. A simple and effective analytical method based on reversed-phased liquid chromatography with fluorescence was developed and validated for the simultaneous determination of eight FQs in wastewater at trace level. Aqueous samples were extracted using AnpelTM MEP cartridges where they were subsequently eluted by formic acid in methanol. The aqueous extracts were analyzed by gradient elution Liquid Chromatography with Fluorescence Detection (LC–FLD), whose mobile phase was composed of acetonitrile and 10 mM tetrabutyl ammonium bromide (TBAB). The limits of detection (LOD) and the relative standard deviation (RSD) were as low as 0.11–1.06 μg/L and 2–5%, respectively. The presented method was successfully applied to quantify FQs in the influent and effluent of several typical Sewage Treatment Plants (STPs) in Shanghai. For the extraction of 100 mL influent and 500 mL effluent sewage water samples, recoveries obtained were between 79–109% and 80%–105%, respectively. 7 FQs were occurred and identified in the STPs with the concentrations varying from 7 ng/L to 1 μg/L. Norfloxacin, ciprofloxacin and lomefloxacin were the most frequently detected antibiotics occurring in the wastewaters. The analytical procedure developed may be used for more in-depth studies on the occurrences and the fate of these commonly used pharmaceuticals in the sewage treatment plants and in the aquatic environment.


2004 ◽  
Vol 87 (3) ◽  
pp. 664-670 ◽  
Author(s):  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
José L Tadeo

Abstract A method was developed for the determination of thiabendazole (TBZ) in orange juice and rind based on matrix solid-phase dispersion (MSPD). TBZ was extracted with ethyl acetate and the extract was subsequently cleaned up on a solid-phase extraction column. Fungicide residues were determined by liquid chromatography with fluorescence detection. Recoveries through the method ranged from 87 to 97% with relative standard deviations ≤11%. The detection and quantitation limits were 0.15 and 0.50 μg/kg, respectively. The confirmation of TBZ residues in positive samples was performed by solid-phase microextraction followed by gas chromatography with mass spectrometric detection using selected ion monitoring. The developed method was applied to determine TBZ levels in commercial orange juices and in juice and rind of fresh oranges. The influence of storage and washing of fruits on TBZ residues was also studied.


2013 ◽  
Vol 781-784 ◽  
pp. 942-946 ◽  
Author(s):  
Jian Chao Deng ◽  
Xian Qing Yang ◽  
Lai Hao Li ◽  
Jian Wei Cen ◽  
Shu Xian Hao ◽  
...  

A new method of determination of malachite green (MG) in sediment has been developed by high performance liquid chromatography with fluorescence detection (HPLC-FLD). It is based on use of a deoxidation reaction which converts malachite green (MG) into LMG in the process of extraction. The sediment samples were extracted with a solution of formic acid and acetonitrile. Clean up and isolation was performed on MCX solid phase extraction (SPE) column. Chromatographic separation was achieved by using C18column with an isocratic mobile phase consisting of acetonitrile and ammonium acetate buffer (0.05 M, pH 4.5) (80:20, v/v). High performance liquid chromatography with fluorescence detector (λex=265 nm and λem=360 nm) was used for the determination of LMG. The recovery values of MG in sediment samples fortified with MG were determined by measuring the amount of MG in the samples, after carrying out deoxidation reaction with potassium borohydride, which converts the MG into LMG. Under the optimized conditions, the average recoveries of MG from sediment at three levels (1.0, 10 and 50 μg/kg) were 85.0% (range from 80.8 to 87.6%). Relative standard deviations (RSD) of recoveries at all fortification levels were less than for 9.57% for MG. The method detection limit obtained for MG was 0.5 μg/kg.


2000 ◽  
Vol 83 (1) ◽  
pp. 20-25 ◽  
Author(s):  
Wenhong Luo ◽  
Catharina Y W Ang

Abstract Trace levels of amoxicillin residues were determined in animal tissues by liquid chromatography (LC) with fluorescence detection. An improved solid-phase extraction (SPE) procedure requiring less flammable solvent (diethyl ether) was developed for sample preparation. Muscle samples of beef, pork, chicken, and tilapia were extracted with a phosphate buffer followed by the modified SPE procedure for cleanup and concentration prior to the LC–fluorescence analysis. Average recoveries of fortified amoxicillin at 5, 10, and 20 μg/kg ranged from 83.9 to 85.8% in beef, 86.1 to 88.1% in pork, 81.7 to 82.9% in chicken, and 92.5 to 95.4% in tilapia. Relative standard deviations were <4%.


2020 ◽  
Vol 2020 ◽  
pp. 1-12
Author(s):  
Yongping Chen ◽  
Sudong Xia ◽  
Xianqin Han ◽  
Zhiru Fu

A fast-analytical method using simplified extraction has been developed for the simultaneous determination of 42 compounds from 4 different classes of veterinary drugs (amphenicols, triphenylmethane, fluoroquinolones, and sulfonamides) in fish by reverse phase liquid chromatography-tandem mass spectrometry. The selection of extraction reagents was optimized using different types of microfiltration membrane, mobile phase, and LC column. Samples were extracted using 0.4% hydrochloric acid in acetonitrile and ethyl acetate and then were cleaned up using solid-phase extraction Cleanert Alumina N columns (500 mg) and Oasis hydrophilic-lipophilic balance (HLB) cartridges. The chromatographic separation was performed on a XR-ODS C8 column using a mobile phase of (A) 0.1% formic acid and 2 mM ammonium acetate and (B) 0.1% formic acid acetonitrile at a flow rate of 0.25 mL·min−1. The results indicated 67.7–112.8% recovery of 42 compounds with an intra- and interday relative standard deviations less than 10%. The limits of quantification for analytes were in the range of 0.3–1.0 μg kg−1 for samples which were satisfactory to support future surveillance monitoring. The method applicability was checked by analyzing 30 fish samples collected from local markets. Two fish samples surpassed the established MRL of 100 μg kg−1 with values of 104 μg kg−1 and 112 μg kg−1.


2019 ◽  
Vol 58 (2) ◽  
pp. 98-108 ◽  
Author(s):  
Sibel Yalçın ◽  
Emine Şükran Okudan ◽  
Özge Karakaş ◽  
Ayşe Nur Önem

Abstract Analysis of plant growth regulators (PGRs) should be approached by considering their extremely low concentrations and serious interfering effects that result from the matrix of various plant tissues. In the current research, the separation and simultaneous determination of different classes of phytohormones in 14 seaweeds collected from Turkey seashores were achieved by using solid-phase extraction (SPE) followed by a rapid and sensitive liquid chromatography tandem mass detection method. OASIS HLB (Hydrophilic-Lipophilic Balance) cartridges were successfully used for SPE process to eliminate the matrix effect and enhance the PGRs including zeatin, benzyl amino purine, indole-3-acetic acid, abscisic acid and gibberellic acid within partially different polarities. Based on the optimized experimental conditions, the method presented excellent performance related to linearity (r, 0.9996–0.9999) within the ranges of 0.5–500 ng/mL, relative standard deviation values ((1.43–2.01) for intraday and (2.36–3.50) for interday)), the limit of detection (0.01–0.84 μg/L) and the limit of quantification (0.02–2.76 μg/L). The obtained results confirm that the SPE–liquid chromatography/tandem mass spectrometry method performed is highly effective and convenient for routine analyses of trace amounts of the tested phytohormones in seaweeds and any other plant samples as well.


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