猪肉中19种β-受体激动剂的液相色谱串联四极杆-飞行时间质谱(Q-TOF)筛查和确证方法研究  

Screening and confirmation of 19 β-agonists in pork by high-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry

作　　者：颜春荣[1] 张波 方萍[1] 王多娇[1] 徐春祥[1] 

机构地区：[1]江苏省产品质量监督检验研究院,南京210007 [2]山东省环保技术服务中心,济南270000

出　　处：《分析试验室》2015年第1期35-39,共5页Chinese Journal of Analysis Laboratory

基　　金：江苏省质量技术监督局科技项目(KJ122701)

摘　　要：利用PCDL数据库中准确质量数、保留时间和二级质谱图对猪肉中19种β－受体激动剂进行Q－TOF筛查和确证分析，其匹配度分值均达到97％以上。选择Agilen tZORBAX Eclipse PlusC_18（2．1mm×100mm，1．8μm），以0．1％甲酸溶液和甲醇为流动相进行梯度洗脱，目标物在13min内完成分离。各物质的线性范围为0．5～50．0μg/L，相关系数大于0．994，定量限为0．5ng／g。在空白猪肉样品中添加0．5，5．0，50．0μg/kg的待测物质时，加标回收率为75．2％～107．7％，RSD均小于16％。方法可应用于猪肉中β－受体激动剂的筛查和确证。19 β -agonists in pork were screened and confirmed by accurate mass, retention time and product ion chromatogram in the created PCDL library through high-performance liquid chromatography-quadrupole-time-of- flight mass spectrometry and all the compounds scored higher than 97. The analysts were completely separated in 13 minutes by a Agilent ZORBAX Eclipse Plus C_18 （2. 1 mm × 100 mm, 1.8 μm） column utilizing gradient elution with methanol and water （0. 1% formic）. Results showed good linear relationship over the concentration range of 0. 5 - 50. 0 μg/L with the con＇elation coefficients greater than 0. 994, and the limit of quantitation was 0. 5 ng/g. The average recoveries rates of 19 β-agonists were 75.2% ～ 107.7% when the spiked levels were 0. 5, 5.0 and 50. 0 μg/kg with relative standard deviations（RSD） less than 15.3%. The developed method is applicable for screening and confirmation of 19 β-agonists in pork with the accuracy and conveniences.

关 键 词：β-受体激动剂 液相色谱串联四级杆-飞行时间质谱(Q-TOF) 筛查 确证 

分 类 号：O657.63[理学—分析化学]