Determination of closantel and rafoxanide in animal tissues by online anionic mixed-mode solid-phase extraction followed by isotope dilution liquid chromatography tandem mass spectrometry

• Published in: Journal of separation science Vol. 34; no. 12; pp. 1366 - 1374
• Main Authors: Lai, Shirley Sau Ling, Yeung, Hoi Sze, Lee, Wai On, Ho, Clare, Wong, Yiu Tung
• Format: Journal Article
• Language: English
• Published: Weinheim Wiley-VCH Verlag 01.06.2011; WILEY-VCH Verlag; WILEY‐VCH Verlag; Wiley; Wiley Subscription Services, Inc
• Subjects: Animal Structures - chemistry; animal tissues; Animals; Anionic mixed-mode solid-phase extraction; Anthelmintics - analysis; Anthelmintics - isolation & purification; Biological and medical sciences; Cattle; Chromatography; Chromatography, Liquid - methods; Cleaning; Closantel; Edible; Food industries; food safety; Fundamental and applied biological sciences. Psychology; Indicator Dilution Techniques; Isotope dilution mass spectrometry; isotope dilution technique; Isotopes; Kidney - chemistry; kidneys; Liquid chromatography; liver; Liver - chemistry; Mass spectrometry; Meat and meat product industries; monitoring; Muscles - chemistry; On-line systems; Online; Online clean-up; Quantitative analysis; Rafoxanide; Rafoxanide - analysis; Rafoxanide - isolation & purification; Salicylanilides - analysis; Salicylanilides - isolation & purification; Sheep; solid phase extraction; Solid Phase Extraction - methods; Tandem Mass Spectrometry - methods; Isotope dilution mass spectrometry; Solid phase extraction; Tandem mass spectrometry; Closantel; Chemical analysis; Anthelmintic; Liver; HPLC chromatography; Veterinary medicine; Kidney; Chemical enrichment; Sample preparation; Animal tissues; Beef; Quantitative analysis; Trace analysis; Offals; Coupled method; Online clean-up; Isotope dilution; Mutton; Contamination; Rafoxanide; Residue; Parasiticide; Mixed adsorbent; Mass spectrometry; Anionic mixed-mode solid-phase extraction
• ISSN: 1615-9306; 1615-9314; 1615-9314
• DOI: 10.1002/jssc.201000675

A rapid and high-throughput isotope dilution LC-MS/MS method with online sample pre-concentration and clean-up using anionic mixed-mode SPE was described for the determination of closantel and rafoxanide in edible bovine and ovine tissues. Tissue samples were extracted with acetonitrile and acetone mixture (60:40, v/v). Sample pre-concentration, clean-up and analysis were completed simultaneously with the online MAX SPE LC-MS/MS system. Closantel-¹³C₆ and rafoxanide-¹³C₆ were used as the internal standards to improve the precision of the method. The method was validated with edible ovine and bovine tissues (muscle, kidney and liver) fortified at three different levels. The accuracy and RSD were 86-106% and ≤14%, respectively. This high-throughput method was suitable for routine quantitative analysis of closantel and rafoxanide in food safety surveillance samples.