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| Simultaneous Determination of Six Teicoplanins Residues in Fish Samples by High Performance Liquid Chromatography－Tandem Mass Spectrometry Coupled with QuEChERS Method |
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| DOI： |
| KeyWord:teicoplanins QuEChERS high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） fish samples |
| Author | Institution |
| JIN Hui，ZHAO Cheng，ZHENG Guang-ming，WEI Lin-ting，SHI Xiao-na，LIN Jia-wei，LI Li-chun，SHAN Qi，MA Li-sha，YIN Yi |
1. College of Food Science and Technology，Shanghai Ocean University，Shanghai ，China; 2. Pearl River Fisheries Research Institute，Chinese Academy of Fishery Sciences/Laboratory of Aquatic Product Quality and Safety Risk Assessment，Ministry of Agriculture and Rural |
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| Abstract: |
| A high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） with QuEChERS pretreatment was developed for the simultaneous determination of six teicoplanins in fish samples．The six components in minced fish samples were extracted with acetonitrile－10% trichloroacetic acid（6∶4） mixed solution．Then the extracted supernatant was cleaned up with 100 mg of primary secondary amine（PSA）．Separation of the targets was performed on an Agilent SB C18 chromatographic column（2.1 mm × 100 mm，1.8 μm） by gradient elution，using 0.1% formic acetonitrile and 0.1% formic as the mobile phase A and the mobile phase B，respectively．The six targets were detected in positive ion electrospray ionization mode（ESI+） under multiple reaction monitoring（MRM） mode，then quantified by the internal standard method with polymyxin sulfate B as the internal standard（IS）．Effects of different types and volumes of extraction solvent，different types and dosages of adsorbent on recoveries of six targets were investigated in detail．The matrix effects of six teicoplanins in different fish substrates were evaluated by the ratio of solvent standard curve and matrix-matched standard curve．Under the optimal conditions，six teicoplanins were well separated by HPLC－MS/MS within 4 min．Good linear relationships were obtained for six analytes in the concentration range of 1－100 μg/L，with their correlation coefficients（r2） greater than 0.998．At three spiked levels of 5.0，10.0 and 25.0 μg/kg，the average recoveries for six analytes in different fish samples ranged from 84.3% to 93.3%，with intra-day relative standard deviations（intra－RSDs） and inter-day relative standard deviations（inter－RSDs） not more than 7.0% and 6.2%，respectively．The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.5－2.0 μg/kg and 2.0－5.0 μg/kg，respectively. The established method was applied to the detection of teicoplanins in various fish samples（forty fish samples that were divided into nine varieties，containing carp，crucian，grass carp，chub，silver carp，mandarin fish，tilapia，pseudosciaena crocea，and scophthalmus maximus） by random sampling principle，and no component of teicoplanin was detected in these actual samples．The developed method proved to be simple，sensitive，accurate and reliable，and was suitable for the simultaneous determination of six teicoplanins in fish samples. |
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