Determination of 5 Macrolide Antibiotics in Pufferfish Meat by HPLC-ESI-MS/MS

Abstract

Abstract: A method has been developed for the simultaneous determination of five marcolide antibiotic residues including lincomycin, oleandomycin, erythromycin, tilmicosin and tylosin in pufferfish meat. Five antibiotic residues in samples were extracted into Tris buffer. The extract was cleaned up on an Oasis HLB column. The antibiotic residues were determined and confirmed by LC-MS/MS and quantified by an internal standard method. The calibration curves of 5 antibiotics exhibited good linearity in the concentration range of 0.002－0.050μg/mL with a correlation coefficient range of 0.9977－1.0000. The average recovery rates of the marcolide antibiotics from pufferfish samples at spike levels of 0.002－0.010 mg/kg was 78.9%－109.0% with a relative standard deviation of 1.3%－5.3% for repeatability and with a relative standard deviation of 5.2%－14.5% for reproducibility. The detection limit was 2.0μg/kg for these 5 antibiotics.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), solid phase extraction (SPE), macrolide antibiotics, pufferfish

CLC Number:

R122.1+1

References

[1] 李岩，邵兵，徐锁洪．动物性食品中大环内酯类抗生素残留分析.中国卫生检验杂志，2005，10(15)：1273～1277；
[2] 王炼，杨元，高玲，等．动物性食品中11种兽药残留的高效液相色谱(HPLC)法测定.中国卫生检验杂志，2004，14(3)：276-2781；
[3] 关于发布《动物性食品中兽药最高残留限量》的通知.农牧发(1999)第17号，1999，09，01:1；
2003，23(6)：434～438；
[4] 史向国，钟大放．液相色谱－质谱联用法鉴定必特螺旋霉素中多组分.质谱学报，2003，4(24)：460～463；
[5] PratsC，Francesch R，ArboixM，et al1Determination of tylosin resi2 dues in different animal tissues by high performance liquid chromatog2 raphy.J ChromatogrB，2001，766(1)：57～65；
[6] Juhel-Gaugain M，Anger B，Laurentie M1 Multiresidue chromato 2 graphi cmethod for the determination of macrolide residuesinmuscle byhigh-performance liquidchromatographywithUV detection.J AOAC Int，1999，82(5)：1046～1053
[7] Moran J W，Turner J M，Coleman MR1 Determination of tilmicosin in bovine and porcine sera by liquid chromatography.J AOAC Int，1997，80(6)：1183～1189；
[8] Multiresidue chromatographic method for the determination of macrolide residues in muscle by high-performance liquid chromatography with UV detection. J AOAC Int. 1999 Sep-Oct;82(5):1046-53；
[9] Determination of macrolide antibiotics by liquid chromatography. J Chromatogr A. 2001 Mar 2;910(2):285-90；
[10] Identification and quantification of five macrolide antibiotics in several tissues, eggs and milk by liquid chromatography-electrospray tandem mass spectrometry. J Chromatogr B Biomed Sci Appl. 2001 Apr 5;753(2):189-202；
[11] Simultaneous determination of residual fourteen kinds of beta-lactam and macrolide antibiotics in bovine muscles by high-performance liquid chromatography with a diode array detector. Shokuhin Eiseigaku Zasshi. 2004 Jun;45(3):161-4；
[12] Simultaneous determination of lincomycin and five macrolide antibiotic residues in honey by liquid chromatography coupled to electrospray ionization mass spectrometry (LC-MS/MS). Food Addit Contam. 2006 Nov;23(11):1099-108；
[13] Simultaneous determination of five macrolide antibiotics in meat by high-performance liquid chromatography. J Chromatogr A. 1998 Jul 3;812(1-2):295-302；
[14] An analytical study of antibacterial residues in meat: the simultaneous determination of 23 antibiotics and 13 drugs using gas chromatography. Vet Hum Toxicol. 1992 Oct;34(5):393-7；
[15] 中华人民共和国国家质量监督检验检疫总局,GB/T 20762-2006.中华人民共和国国家标准—畜禽肉中林可霉素、竹桃霉素、红霉素、替米考星、泰乐菌素、克林霉素、螺旋霉素、吉它霉素、交沙霉素残留量的测定方法液相色谱-串联质谱.北京：中国标准出版社，2006-12-28。