Trace analysis of endectocides in milk by high performance liquid chromatography with fluorescence detection

Cerkvenik-Flajs, Vesna; Milčinski, Luka; Süssinger, Adica; Hodošček, Lena; Danaher, Martin; Antonić, Jan

doi:10.1016/j.aca.2010.01.040

Cited by 33 publications

(15 citation statements)

References 20 publications

(34 reference statements)

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“…There are a number of reports published on the highperformance liquid chromatography (HPLC) analysis of MOX as active pharmaceutical ingredients (API), in environmental, food, milk and other encompassing matrices using different extraction and detection methods [6][7][8][9][10][11]. A comprehensive methodology review by Danaher et al on ML outlines details of commonly used techniques for analysis of MOX in biological matrices [12].…”

Section: Introductionmentioning

confidence: 99%

Isolation and characterization of degradation products of moxidectin using LC, LTQ FT-MS, H/D exchange and NMR

et al. 2012

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This study aimed to evaluate the degradation profile and pathways, and identify unknown impurities of moxidectin under stress conditions. During the experiments, moxidectin samples were stressed using acid, alkali, heat and oxidation, and chromatographic profiles were compared with known impurities given in European Pharmacopeia (EP) monograph. Moxidectin has shown good stability under heat, while reaction with alkali produced 2-epi and ∆2,3 isomers (impurities D and E in EP) by characteristic reactions of the oxahydrindene (hexahydrobenzofuran) portion of the macrocyclic lactone. Two new, previously unreported, unknown degradation products, i.e. impurity 1 and impurity 2, detected after acid hydrolysis of moxidectin (impurity 2 was also observed to a lesser extent after oxidation), were isolated from sample matrices and identified using liquid chromatography, NMR, high-resolution FT-ICR MS, and hydrogen/deuterium exchange studies. FTMS analysis showed accurate mass of molecular ion peaks for moxidectin at m/z 640.38412, impurity 1 at m/z 656.37952 and impurity 2 at m/z 611.35684, giving rise to daughter ions traceable up to the seventh levels of MS(n) experiments and supporting the proposed structures. Both unknown impurities along with moxidectin were fully characterized by (1)H, (13)C, 1D HMBC and 2D (NOESY, COSY and HSQC) NMR experiments. The interpretation of experimental data positively identified impurity 1 as 3,4-epoxy-moxidectin and impurity 2 as 23-keto-nemadectin. The identification of new impurities and correlation of their chromatographic profiles with the EP method is very useful to establish the stability profile of moxidectin and its preparations, as well as add value to the forthcoming moxidectin finished product European Pharmacopeia monographs.

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Section: Introductionmentioning

confidence: 99%

Isolation and characterization of degradation products of moxidectin using LC, LTQ FT-MS, H/D exchange and NMR

et al. 2012

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“…Abamectin was suspected causing adverse effects in the aquatic environment, even in low concentrations, as it presents high toxicity to aquatic organisms, such as fish and microcrustaceans (Tisler, Erzen, 2006). Several different methods have been reported in scientific literature for the analyses of abamectin, such as, high performance liquid chromatography (HPLC) (Kulik et al, 2011), liquid chromatography coupled to mass spectrometry (LC-MS) (Valenzuela et al, 2000;Pozo et al, 2003;Yoshii et al, 2004;Xiaolin et al, 2006;Thompson et al, 2009;Rübensam et al, 2011;Tao et al, 2012;Campillo et al, 2013;Ismail et al, 2013), HPLC with fluorescence (Diserens, Henzelin,1999;Souza et al, 2003;Kolar et al, 2004;Borges et al, 2008;Cerkvenik-Flajsa et al, 2010;Xie et al, 2011;Rahman et al, 2013), and UHPLC with fluorescence (Liu et al, 2001;Romero-González et al, 2011). The aim of this research was to validate a HPLC method for quantitative determination of abamectin homologs (H 2 B 1a and H 2 B 1b ) in gel formulation, as this drug is widely used in veterinary practice.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of abamectin homologs H 2 B 1a and H 2 B 1b in gel formulation by high performance liquid chromatography

Alexandre

Aurora-Prado

Mariño

et al. 2016

Braz. J. Pharm. Sci.

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Abamectin is a drug with antiparasitic properties used in several pharmaceutical formulations. The objective of this research was to develop and validate a high performance liquid chromatographic (HPLC) method for quantification of the two abamectin homologs (H 2 B 1a and H 2 B 1b) in gel formulation. This HPLC method was validated using a LichroCart ® 100 RP-18 (125 x 4 mm, 5 µm) column. The mobile phase contained of acetonitrile and water (95:5 v/v) with 1% acetic acid. The flow rate was 1.0 mL min-1 and UV detection was performed at 245 nm. Mobile phase solutions were prepared containing a nominal concentration 185.2 µg mL-1 H 2 B 1a and 9.6 µg mL-1 H 2 B 1b. The method displayed good linearity in the concentration range of 148.1-222.3 µg mL-1 and 7.7-11.5 µg mL-1 , for H 2 B 1a and H 2 B 1b , respectively, with a correlation coefficient of (r)> 0.99 for both compounds, calculated by the least mean squares method. Detection limits (DLs) were 2.8 µg mL-1 and 1.2 µg mL-1 and quantitation limits (QLs) were 8.6 µg mL-1 and 3.8 µg mL-1 , for H 2 B 1a and H 2 B 1b , respectively. The method is simple, economical and efficient for the quantitative determination of abamectin H 2 B 1a and H 2 B 1b homologs in pharmaceutical preparations. Uniterms: Abamectin homologs/validation method/gel formulation. Abamectin homologs. High Perfomance Liquid Chromatography (HPLC).

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“…From a number of multiresidue methods for the determination of residues of macrocyclic lactones in animal tissues or products of animal origin, which have been published (1,8,16,17), only a few are applicable in the analysis of milk samples (3,18).…”

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confidence: 99%

Control of Residues of Five Macrocyclic Lactones in Cow Milk By Liquid Chromatography with Fluorescence Detection

Szprengier-Juszkiewicz

Jedziniak

Olejnik

et al. 2012

Bulletin of the Veterinary Institute in Pulawy

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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.

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Trace analysis of endectocides in milk by high performance liquid chromatography with fluorescence detection

Cited by 33 publications

References 20 publications

Isolation and characterization of degradation products of moxidectin using LC, LTQ FT-MS, H/D exchange and NMR

Isolation and characterization of degradation products of moxidectin using LC, LTQ FT-MS, H/D exchange and NMR

Simultaneous determination of abamectin homologs H 2 B 1a and H 2 B 1b in gel formulation by high performance liquid chromatography

Control of Residues of Five Macrocyclic Lactones in Cow Milk By Liquid Chromatography with Fluorescence Detection

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