Citation: CHEN Xinglian, LIN Tao, LIU Xingyong, MEI Wenquan, YANG Dongshun, LI Yangang, LI Maoxuan, WANG Luxiang. Simultaneous determination of antibiotics and triphenylmethanes veterinary drug residues in fish and shrimp by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(9): 946-954. doi: 10.3724/SP.J.1123.2019.02016 shu

Simultaneous determination of antibiotics and triphenylmethanes veterinary drug residues in fish and shrimp by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry

1.
Quality Standardizing and Testing Technology Institute, Yunnan Academy of Agricultural Sciences, Kunming 650224, China;
2.
Supervision & Testing Center for Farm Products Quality, Ministry of Rural Agriculture(Kunming Section), Kunming 650224, China

Received Date: 28 February 2019

Fund Project: Science and Technology Project of Yunnan Science and Technology Department (Major Special Project) (No. 2018BC005-04).

A method was established to rapidly determine 20 kinds of veterinary drug residues including three catagories of antibiotics (sulfonamides, quinolones, and chloramphenicols) and two kinds of triphenylmethanes (malachite green (MG) and leucomalachite green (LMG)) in fish and shrimp, based on dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry. The samples were first hydrolyzed using a dipotassium hydrogen phosphate solution, and then extracted using acetonitrile. Afterward, the extraction solution was dehydrated and salted out with sodium chloride and condensed to nearly dry using a rotating evaporator. This residue was dissolved in 1.0 mL methanol. The resulting solution was purified by dispersive solid phase extraction method with C18 and PSA sorbents, and filtered through a filter. The target compounds were separated employing a ZORBAX C18 column. The mass spectrometer datas were acquired by multiple reaction monitoring (MRM) of positive and negative modes and quantitated applying the isotope internal standard method. The 20 veterinary drugs showed a good linear relationship in the range of 0.2-300 μg/L. The limits of detection and the limits of quantification were 0.1-0.6 and 0.3-1.8 μg/kg, respectively, while the correlation coefficients were greater than 0.99. The average recoveries at the three spiked levels (1, 5, and 20 times of quantitative limits) ranged between 72.5%-118%, with the relative standard deviations of 1.9%-9.8%. The advantages of method include a simple pretreatment, a high detection efficiency, and a low cost. Moreover, it is suitable for the simultaneous determination of multiple veterinary drug residues in fish and shrimp.
- dispersive solid phase extraction (DSPE),
- ultra high performance liquid chromatography (UHPLC),
- tandem mass spectrometry (MS/MS),
- antibiotics,
- triphenylmethanes,
- fish,
- shrimp,
- veterinary drug residue
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沈阳化工大学材料科学与工程学院沈阳 110142