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超高效液相色谱-串联质谱法测定牛肉中9种头孢菌素类药物残留
其他题名Determination of 9 cephalosporin drug residues in beef by ultra performance liquid chromatography-tandem mass spectrometry
白国涛1; 储晓刚2; 潘国卿1; 李秀琴2; 雍伟2
ISSN1000-8713
出版年2009
卷号27期号:4页码:417-420
中文摘要建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定牛肉中9种头孢菌素类药物残留的方法.头孢菌素类药物经乙腈-水溶液提取,Oasis HLB柱净化.以乙腈-水(含0.05%甲酸)为流动相,UPLC-MS/MS法测定.结果表明,9种头孢菌素类抗生素在 5 min 内达到分离.头孢呋辛的定量限为10 mug/kg,头孢洛宁和头孢噻夫的定量限为0.5 mug/kg,其他头孢菌素的定量限均为1.0 mug/kg.加标回收率为74.2% ~119% ,精密度(RSD)≤15% .该方法简单、灵敏、可靠,适用于牛肉中头孢菌素类药物残留的分析确证.
英文摘要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 ℃ 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 ℃ 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 UPLCTM 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 mug/kg,respectively;the LOQs of other cephalosporins were 1.0 mug/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.
中文关键词超高效液相色谱-串联质谱 ; 头孢菌素类药物 ; 牛肉
英文关键词ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) cephalosporin beef
语种中文
国家中国
收录类别CSCD
WOS类目CHEMISTRY ANALYTICAL
WOS研究方向Chemistry
CSCD记录号CSCD:3689263
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/223995
作者单位1.内蒙古出入境检验检疫局, 呼和浩特, 内蒙古 010020, 中国;
2.中国检验检疫科学研究院, 北京 100025, 中国
推荐引用方式
GB/T 7714
白国涛,储晓刚,潘国卿,等. 超高效液相色谱-串联质谱法测定牛肉中9种头孢菌素类药物残留[J],2009,27(4):417-420.
APA 白国涛,储晓刚,潘国卿,李秀琴,&雍伟.(2009).超高效液相色谱-串联质谱法测定牛肉中9种头孢菌素类药物残留.,27(4),417-420.
MLA 白国涛,et al."超高效液相色谱-串联质谱法测定牛肉中9种头孢菌素类药物残留".27.4(2009):417-420.
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