摘要
建立一个超高压液相色谱．串联三重四极杆质谱法快速测定乳制品中氯霉素，甲砜霉素，氟甲砜霉素的方法。样品中目标物经乙腈溶液提取，正己烷脱脂后，经中性氧化铝固相萃取小柱纯化，在ZORBAXSB—C18色谱柱上，以水-乙腈体系为流动相，采用梯度洗脱，流速为0．3mL／min，进样量10μL，经UPLC—MS／MS（MRM模式监测，负离子模式扫描）检测后内标法峰面积定量。结果表明：在0．1～8．0ng／mL范围内该方法线性良好，R^2均大于0．998，不同基质样品各组分回收率在85％～110％之间，方法定量限均在0．06μg／kg以下，灵敏度足以满足乳制品检测的需要。
A method for the rapid determination of chloramphenicol, thiamphenicol and florfenicol in dairy products by ultra-high pressure liquid chromatography -tandem triple quadrupole mass spectrometry was developed. Target samples extracted by acetonitrile, degreased by hexane and purified by a neutral alumina solid phase extraction column were separated on a ZORBAX SB-CI8 column with water - acetonitrile system as the mobile phase using gradient elution at a flow rate of 0. 3 mL/min with the sample amount of 10 μL and detected by UPLC-MS/MS （in MRM mode with monitoring negative ion） with the external standard method. The results showed good linearity in the range from 0. 1 to 8.0ng/mL with R^2 ≥ 0. 998 and recoveries for each component at different matrices were between 85% and 110%, LOQ of the method were below 0. 06 μg/kg and the sensitivity was sufficient to meet the needs for the detection of dairy products.
出处
《分析试验室》
CAS
CSCD
北大核心
2013年第12期101-105,共5页
Chinese Journal of Analysis Laboratory
