基于热解吸低温等离子体质谱技术快速筛查饲料中瘦肉精

Rapid Screening of Lean Meat Essence in Feed by Low Temperature Plasma Mass Spectrometry

  • 摘要: 本研究建立了热解吸低温等离子体离子源结合飞行时间质谱(TD-LTP-MS)法,快速筛查饲料中西马特罗、特布他林、西布特罗、克伦特罗、马布特罗、马贲特罗等6种瘦肉精。样品经简单的前处理后,在正离子模式下进行分析。结果表明,在热解吸温度210 ℃、氦气流速1.0 L/min条件下,6种瘦肉精在5~500 μg/kg浓度范围内的线性关系良好,相关系数R大于0.992,检出限均低于3.1 μg/kg,加标回收率在71.4%~119.2%之间。该方法相较于现行的国标,具有样品前处理简单、检测速度快、结果符合筛查要求等特点,适用于饲料中瘦肉精的高通量快速筛查。

     

    Abstract: Clenbuterol, also known as lean meatines, is a β-stimulant hormone. Lean meatiness will promote animal growth and increase lean meat rate, which has been widely used as feed additive. However, the overuse of lean meatiness often forms residues in animals, and human consumption of lean meat essence residues can lead to acute poisoning, organ damage and even life-threatening. Although clenbuterol has long been banned in China, it is still used secretly by many merchants for profit. The production, sale and use of "lean meat essence" not only endanger the health of the people, but also endanger the sustainable and healthy development of aquaculture and social stability. Therefore, the development of rapid and effective detection methods to regulate the market can effectively prevent such things. A method of thermal analysis of low temperature plasma ion source combined with time of flight mass spectrometry (TD-LTP-MS) was developed for rapid screening of six lean meatines (simaterol, terbutaline, sebuterol, clenbuterol, malbuterol, and machaterol) in feed. Helium flow rate and thermal desorption temperature are important factors to determine the performance of low temperature plasma ion source. Increasing the helium flow rate can increase the active substances such as Hem and N2+, thus improving the ionization effect. The lean meatines veterinary medicine generally has the higher boiling point, so higher thermal desorption temperature is advantageous to desorb them from the solvent. In this study, the low temperature plasma ion source conditions were optimized in the range of helium flow rate of 0.3-1.9 L/min and thermal desorption temperature of 160-260 ℃. Finally, the helium flow rate of 1.0 L/min and thermal desorption temperature of 210 ℃ were the optimum condition for the ionization of six kinds lean meatines. The sample was extracted by 10 mL 0.1% acetonitrile oscillation for 5 min and then centrifuged at 2 500 r/min for 2 min. The supernatant was added 250 mg PSA and 50 mg C18 to purify the sample. The final sample was analyzed by TD-LTP-MS method in positive ion mode. Results showed that there were good linear relationships for the 6 analytes in the range of 5-500 μg/kg with the correlation coefficients greater than 0.992. The detection limits were lower than 3.1 μg/kg and the recovery rate was 71.4%-119.2%. The method is simple and fast, without tedious pretreatment, and is suitable for high-throughput screening of lean meatine in feed.

     

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