超高效液相色谱-串联质谱法同时测定牛肉中18种食源性兴奋剂类药物残留

引用本文: 齐鹤鸣, 韩深, 吕美玲, 尹志强, 严华, 李建辉, 崔凤云. 超高效液相色谱-串联质谱法同时测定牛肉中18种食源性兴奋剂类药物残留[J]. 色谱, 2018, 36(7): 621-628. doi: 10.3724/SP.J.1123.2018.01024 shu

Citation: QI Heming, HAN Shen, LÜ Meiling, YIN Zhiqiang, YAN Hua, LI Jianhui, CUI Fengyun. Simultaneous determination of 18 food-borne stimulant drug residues in beef using ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(7): 621-628. doi: 10.3724/SP.J.1123.2018.01024 shu

超高效液相色谱-串联质谱法同时测定牛肉中18种食源性兴奋剂类药物残留

齐鹤鸣 ^1, ,
韩深 ^1, ,
吕美玲 ^2, ,
尹志强 ^1, ,
严华 ^1, ,
李建辉 ^1, ,
崔凤云 ^1,

1.
北京出入境检验检疫局检验检疫技术中心, 北京 100026;
2.
安捷伦科技(中国)有限公司, 北京 100102
基金项目:
国家质量监督检验检疫总局科技计划项目（2017IK143，2016IK018，2016IK021）.

摘要: 建立了超高效液相色谱-串联质谱（UHPLC-MS/MS）检测牛肉中18种食源性兴奋剂类药物残留的方法。牛肉组织经酸化乙腈提取，Captiva小柱脱脂净化后，用无水硫酸镁干燥，上清液氮吹浓缩，残渣用甲醇-水（7：3，v/v）溶解。采用Agilent Zorbax Phenyl-Hexyl色谱柱分离，以5 mmol/L醋酸铵水溶液（含0.01%（v/v）醋酸）和甲醇-乙腈（7：3，v/v）作为流动相进行梯度洗脱，在电喷雾正负离子切换模式下以多反应监测（MRM）方式检测，用基质匹配标准曲线外标法定量。结果表明，18种食源性兴奋剂类药物在0.10~50 μg/L范围内线性关系良好，相关系数（R²）≥ 0.9950；在0.4、1.0和2.0 μg/kg添加水平下的回收率为57.3%~117.5%，相对标准偏差为3.1~15.6%（n=5）；方法的检出限和定量限分别为0.0006~0.0900 μg/kg和0.0020~0.3000 μg/kg。该法可以实现对牛肉样本中18种兴奋剂类药物残留的定性定量分析，具有简单、快速、准确性高的特点。

关键词:

English

Simultaneous determination of 18 food-borne stimulant drug residues in beef using ultra-high performance liquid chromatography-tandem mass spectrometry

1.
Inspection and Quarantine Technique Center, Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China;
2.
Agilent Technologies(China) Limited, Beijing 100102, China
Received Date: 14 January 2018
Fund Project:
Science and Technology Planning Project of General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China(Nos. 2017IK143, 2016IK018, 2016IK021).

Abstract: A method for the simultaneous determination of 18 food-borne stimulant drug residues in beef was developed based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The beef sample was extracted with acidified acetonitrile, cleaned up by Captiva filtration cartridge. The extract was dried with anhydrous magnesium sulfate, and then concentrated by nitrogen flow. The obtained residue was re-dissolved in methanol-water (7:3, v/v). The separation was performed on an Agilent Zorbax Phenyl-Hexyl column with 5 mmol/L ammonium acetate solution (containing 0.01% (v/v) acetic acid) and methanol-acetonitrile (7:3, v/v) as mobile phases with gradient elution. The analyte was detected in positive and negative ion modes and the multiple reaction monitoring (MRM) mode. The quantification analysis was performed by external standard method using matrix-matched calibration curves. The method was linear with the correlation coefficients (R²) ≥ 0.9950 in the range of 0.10-50 μg/L. At the spiked levels of 0.4, 1.0 and 2.0 μg/kg, the recoveries of all compounds ranged from 57.3% to 117.5%, with RSDs in range of 3.1%-15.6% (n=5). The limits of detection and limits of quantification were in the range of 0.0006-0.0900 μg/kg and 0.0020-0.3000 μg/kg, respectively. The method is simple, rapid, accurate and sensitive, and can meet the requirement for the determination of the 18 food-borne stimulant drug residues in beef.

Key words:

ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)
/ food-borne stimulant drug
/ residues
/ beef tissue

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超高效液相色谱-串联质谱法同时测定牛肉中18种食源性兴奋剂类药物残留

English

Simultaneous determination of 18 food-borne stimulant drug residues in beef using ultra-high performance liquid chromatography-tandem mass spectrometry

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中国化学会秘书处

超高效液相色谱-串联质谱法同时测定牛肉中18种食源性兴奋剂类药物残留

English

Simultaneous determination of 18 food-borne stimulant drug residues in beef using ultra-high performance liquid chromatography-tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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