食品科学 ›› 2021, Vol. 42 ›› Issue (14): 276-285.doi: 10.7506/spkx1002-6630-20200624-329

• 安全检测 • 上一篇    下一篇

超高效液相色谱-四极杆/飞行时间质谱检测猪肉和牛肉中30 种食源性兴奋剂类药物残留

马俊美,范素芳,李强,何亮娜,范力欣,曹梅荣,孙磊,王东,孙文毅   

  1. (河北省食品检验研究院,河北省食品安全重点实验室,河北 石家庄 050091)
  • 发布日期:2021-07-27
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1603400);河北省市场监管局科技计划项目(2020ZD06)

Determination of 30 Foodborne Stimulant Drug Residues in Pork and Beef Using Ultra-high Performance Liquid Chromatography Coupled with Quadrupole-Time of Flight Mass Spectrometry

MA Junmei, FAN Sufang, LI Qiang, HE Liangna, FAN Lixin, CAO Meirong, SUN Lei, WANG Dong, SUN Wenyi   

  1. (Key Laboratory of Food Safety of Heibei Province, Hebei Food Inspection and Research Institute, Shijiazhuang 050091, China)
  • Published:2021-07-27

摘要: 建立猪肉和牛肉中30 种食源性兴奋剂的超高效液相色谱-四极杆/飞行时间质谱的快速筛查和确证方法。样品经37 ℃酶解16 h,体积分数1.0%甲酸-乙腈溶液提取后,经PRiME-HLB通过式固相萃取小柱净化,用Waters XBridge BEH C18柱分离,在飞行时间质谱模式和数据依赖扫描串联质谱模式对目标物进行检测,通过一次数据采集,可同时完成化合物的定性筛查和确证。结果表明:30 种食源性兴奋剂的精确质量数偏差小于5.0×10-6,在0.5~100.0 ng/mL范围内线性良好,相关系数大于0.998 0。检出限范围为0.1~2.0 μg/kg;定量限范围为0.2~4.0 μg/kg。方法回收率范围为77.99%~109.2%,相对标准偏差为0.29%~9.68%(n=6)。该方法有效提高了食源性兴奋剂检测的效率和准确度,具有较强的实用价值。

关键词: 超高效液相色谱-四极杆/飞行时间质谱;猪肉;牛肉;食源性兴奋剂

Abstract: A new rapid method for screening and identification of 30 foodborne stimulant drug residues in pork and beef by ultra-high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS) was developed. The samples were enzymatically digested for 16 h at 37 ℃ and extracted with acetonitrile (containing 0.10% formic acid, V/V), and the extract was cleaned up using a PriME-HLB cartridge, and then separated on a Waters XBridge BEH C18 column by gradient elution. The analytes were detected by time of flight mass spectrometry-tandem mass spectrometry (TOF/MS) and information dependent acquisition-tandem mass spectrometry (IDA-MS/MS), and they were qualitatively screened and confirmed in one data acquisition cycle. The results showed that the mass accuracy errors of the 30 foodborne stimulant drug residues were lower than 5.0 × 10-6. Good linearity in the range of 0.5–100.0 ng/mL were observed for the analytes, with correlation coefficients greater than 0.998 0. The limits of detection were in the range of 0.1–2.0 μg/kg and the limits of quantitation were in the range of 0.2–4.0 μg/kg. The recoveries of the developed method were in the range of 77.99%–109.2%, with relative standard deviations of 0.29%–9.68% (n = 6). This method proved to efficient and accurate and could have great practical value.

Key words: ultra-high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry; pork; beef; foodborne stimulant drugs

中图分类号: