食品科学

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HPLC-q/LTQ-MS法测定肉及肉制品中10 种β-受体激动剂

张 旖,赵善贞*,曲 栗,曹 晨,时逸吟,伊雄海   

  1. 上海出入境检验检疫局,上海 200135
  • 出版日期:2014-10-25 发布日期:2014-11-07
  • 基金资助:

    上海出入境检验检疫局科研项目(HK014-2014;HK008-2014);
    国家质量监督检验检疫总局质检公益性行业科研专项(201110019-04;201310140-02);
    国家重大科学仪器设备开发专项(2013YQ15055705)

Determination of 10 Kinds of β-Agoinsts in Meat and Meat Products by Matrix Solid-phase Dispersion-High Performance Liquid Chromatography Tandem Quadrupole Linear Ion Trap Mass Spectrometry

ZHANG Yi, ZHAO Shan-zhen*, QU Li, CAO Chen, SHI Yi-yin, YI Xiong-hai   

  1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Online:2014-10-25 Published:2014-11-07

摘要:

建立基质分散固相萃取-高效液相色谱-四极杆串联线性离子阱质谱法快速测定肉和肉制品中的克仑特罗、沙丁胺醇、莱克多巴胺、特布他林、妥布特罗、氯丙那林、喷布特罗、西马特罗、非诺特罗以及苯乙醇胺A 10 种β-受体激动剂。猪肉、肠衣和午餐肉中的β-受体激动剂经乙腈提取后,采用基质分散固相萃取净化,内标法定量。方法按照多反应监测、信息相关采集、增强离子扫描,结合10 种β-受体激动剂标准的子离子谱库检索进行分析,可对试样中10 种β-受体激动剂同时进行定性、定量测定。结果表明,克仑特罗在0.05~0.5 ng/mL质量浓度范围内,其余9 种药物残留在0.5~5 ng/mL质量浓度范围内线性良好,相关系数(r2)均大于0.99。克仑特罗定量限为0.05 μg/kg,其余9 种药物定量限为0.5 μg/kg。10 种β-受体激动剂在猪肉、肠衣和午餐肉中平均回收率分别在85.6%~118.4%、85.6%~119.2%、80.4%~118.4%之间(n=6),相对标准偏差在1.47%~14.4%、2.45%~15.4%、1.04%~12.5%之间(n=6)。方法可对猪肉、肠衣、午餐肉等肉和肉制品中10 种β-受体激动剂药物的定性同时进行定量测定。

关键词: &beta, -受体激动剂, 基质分散固相萃取, 高效液相色谱-四极杆-线性离子阱质谱, 肉与肉制品

Abstract:

A method based on matrix solid-phase dispersion-high performance liquid chromatography tandem quadrupole
linear ion trap mass spectrometry (HPLC-q/LTQ-MS) for the determination of 10 kinds of β-agoinsts in meat and meat
products was presented. Clenbuterol, salbutamol, ractopamine, tulobuterol, terbutaline, clorprenaline, penbutolol, cimaterol
and fenoterol were extracted with acetonitrile, followed by a further clean-up procedure using QuEChERS method. A
multiple reaction monitoring (MRM) as survey scan and an enhanced product ion (EPI) scan as dependent scan were
performed in an information dependent acquisition (IDA) experiment. The identification of the compounds was carried out
by library search with a precursor ion MS-MS library based on EPI spectra at three different collision energies in a positive
mode. The results showed that clenbuterol was in the range of 0.05–0.5 ng/mL, and 9 other kinds of β-agoinsts residues were
in the range of 0.5–5 ng/mL with correlation coefficients (r2) higher than 0.99. The limit of quantification was 0.05 μg/kg for
clenbuterol and 0.5 μg/kg for 9 other kinds of β-agoinsts. The recoveries of spiked standards in pork, casing and luncheon
meat ranged from 85.6% to118.4%, 85.6% to119.2%, and 80.4% to 118.4%, with relative standard deviation (RSD) of
1.47%–14.4%, 2.45%–15.4%, and 1.04%–12.5% (n = 6), respectively. This method can be used for simultaneous analysis of
10 kinds of β-agonists in meat and meat products.

Key words: β-agoinsts, matrix solid-phase dispersion, high performance liquid chromatography tandem quadrupole linear ion trap mass spectrometry (HPLC-q/LTQ-MS), meat and meat products

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