[Determination of 9 cephalosporin drug residues in beef by ultra performance liquid chromatography-tandem mass spectrometry].
A confirmative method to determine 9 cephalosporin residues in beef by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The sample was homogenized and extracted with acetonitrile and water for 1 min at 14,000 r/min, centrifuged at 10,000 r/min and 4 degrees C for 10 min. A total of 2 mL saturated sodium chloride solution was added to avoid foaming during the acetonitrile evaporation, the acetonitrile was evaporated below 37 degrees C using a rotary evaporator, and then cleaned up on an Oasis HLB (500 mg, 6 mL) SPE column by washing with 5 mL water and eluting with acetonitrile-water (7:3, v/v). The eluate was blown to dryness under a stream of nitrogen and adjusted to 3.0 mL with water. The separation was carried out on an ACQUITY UPLC BEH C18 column within 5 min, analyzed by UPLC-MS/MS system with external standard method. The limits of quantification (LOQs) of cefuroxime, ceftiofur and cefalonium were 10, 0.5 and 0.5 microg/kg, respectively; the LOQs of other cephalosporins were 1.0 microg/kg. The recoveries of cephalosporins ranged from 74.2% to 119% and the relative standard deviations (RSDs) ranged from 2.9% to 15% for the spiked beef sample. The method is quick, easy, very sensitive and suitable for the determination of cephalosporin residues in beef.
Bai
Guotao
G
Inner Mongolia Entry-Exit Inspection and Quarantine Bureau, Hohhot, China.
Chu
Xiaogang
X
Pan
Guoqing
G
Li
Xiuqin
X
Yong
Wei
W
D000818:Animals; D002417:Cattle; D002444:Cefuroxime / Q000032:analysis; D002511:Cephalosporins / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis; D008460:Meat / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
D002511:Cephalosporins; C053503:ceftiofur; C059979:cefaloram; D002444:Cefuroxime