摘要
建立了一种固相分散萃取-超高效液相色谱-串联质谱(QuEChERS-UPLC-MS/MS)同时检测火锅食材中11种喹诺酮类药物的方法。样品用5%甲酸乙腈溶液提取后加入盐析剂分层,提取液中加入C18和PSA填料进行基质分散固相净化,浓缩后经Poroshell 120EC-C18柱分离,用电喷雾离子源正离子多反应监测(MRM)模式串联质谱进行检测。11种药物在1.0～100.0μg/kg范围内具有较好的线性关系,相关系数均大于0.998。该方法检出限(LOD)为1.8～3.1μg/kg,定量限(LOQ)为6.0～10.3μg/kg。11种药物的回收率为70.1%～100.3%,相对标准偏差(RSD)为2.42%～10.88%。该方法简便快速、灵敏度高、准确度好、使用范围广,可作为火锅食材中11种喹诺酮类药物残留的确证方法。
A method for the simultaneous determination of the residues of 11 quinolones in hot- pot ingredients by quick, easy, cheap, effective, rugged and safe （QuEChERS） extraction and ultra performance liquid chromatography-tandem mass spectrometric method （UPLC-MS/MS） was established. The sample was extracted with acetonitrile （containing 5% formic acid） and followed by stratifying with a salting-out agent. Clean-up of the extracts was processed by C18 and PSA, a modified QuEChERS procedure. The analytes were then separated on a Poroshell 120 EC-Cl8 column, and finally detected by tandem mass spectrometry in positive ESI mode. The linearity of all the I 1 quinolones in the range from I. 0 to 100.0 g/kg had correlation coef- ficients greater than 0. 998. The limits of detection （LOD） of the method were from 1.8 to 3. ! g/kg and the limits of quantification （LOQ） were from 6.0 to 10. 3 ig/kg. The average recov- eries of the 11 quinolones were in the range from 70. 1% to 100.3%, with relative standard devi- ations from 2.42% to 10.88%. The established method is sensitive and of good recoveries. It can be applied as a rapid and reliable method for the determination of the I l quinolones in hot-pot, ingredients.
出处
《色谱》
CAS
CSCD
北大核心
2013年第9期862-868,共7页
Chinese Journal of Chromatography
基金
山东检验检疫局科技计划项目(SK201173)
烟台市科技发展计划项目(2011052)
关键词
分散固相萃取
超高效液相色谱-串联质谱
喹诺酮类药物
火锅食材
QuEChERS
ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）
quinolones
hotpot ingredients
