Volume 9 Issue 4
Aug.  2013
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LUO Fangfang, QIAN Zhuozhen, LIN Rongxiao, WU Chengye. Determination of colistin sulfate, bacitracin and virginiamycin M1 residues in aquatic products by HPLC-MS/MS[J]. South China Fisheries Science, 2013, 9(4): 62-68. DOI: 10.3969/j.issn.2095-0780.2013.04.011
Citation: LUO Fangfang, QIAN Zhuozhen, LIN Rongxiao, WU Chengye. Determination of colistin sulfate, bacitracin and virginiamycin M1 residues in aquatic products by HPLC-MS/MS[J]. South China Fisheries Science, 2013, 9(4): 62-68. DOI: 10.3969/j.issn.2095-0780.2013.04.011
shu

Determination of colistin sulfate, bacitracin and virginiamycin M1 residues in aquatic products by HPLC-MS/MS

  • 1.

    College of Biology Engineering, Jimei University, Xiamen 361021, China

  • 2.

    Fisheries Research Institute of Fujian, Xiamen 361012, China

  • 3.

    Fujian Agriculture and Forestry University, Fuzhou 350002, China

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  • Received Date: October 11, 2012
  • Revised Date: December 28, 2012
    Graphical Abstract
    • Abstract

  • A high performance liquid chromatography tandem mass spectrometric (HPLC-MS/MS) method was established to simultaneously detect colistin sulfuric (CS), bacitracin (BTC) and virginiamycin M1 (VGMM1) in aquatic products. We extracted the samples with methanol-0.1% formicacid(V : V=2 : 5), removed their protein with 4% TCA acetonitril, removed fat with acetonitrile saturated n-hexane, and then cleaned them up with OASiS HLB solid phase extraction (SPE) column. Next, we detected the analytes by HPLC-MS/MS under the selected reaction monitoring mode and quantified them by external standard method. Results show that CS and BTC have good linearity between the peak areas in concentrations ranged 0.01~10.00 mg · L-1, VGMM1 as well in concentrations ranged 0.002~2.000 mg · L-1, and the correlation coefficients (R2) are all more than 0.995. The detection limits of CS, BTC and VGMM1 are 10 μg · kg-1, 10 μg · kg-1and 2 μg · kg-1 respectively, and the quantification limits are 20 μg · kg-1, 20 μg · kg-1 and 4 μg · kg-1respectively. Three samples in three different concentration levels are chosen for recovery, getting a 72.3%~103.9% average recovery rate, and a relative standard deviations varying from 1.10%~10.92%. In conclusion, method proposed has advantages of simplicity, sensitivity and repeatability, which provide technical support for the detection of these 3 kinds of drug residues in aquatic products.

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    • References (17)
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