色谱

色谱 ›› 2015, Vol. 33 ›› Issue (11): 1199-1204.DOI: 10.3724/SP.J.1123.2015.06016

• 技术与应用 • 上一篇    下一篇

QuEChERS-超高效液相色谱-高分辨串联质谱技术检测鸡肉中6种抗球虫药物

木合他拜尔1, 严华2, 徐姗2, 冯楠3, 郝杰3, 朱尘琪1, 郭爽1, 张朝晖2, 韩南银1   

  1. 1. 北京大学药学院, 北京 100191;
    2. 北京出入境检验检疫局检验检疫技术中心, 北京 100026;
    3. 北京市食品安全监控和风险评估中心, 北京 100041
  • 收稿日期:2015-06-10 出版日期:2015-11-08 发布日期:2012-05-30
  • 通讯作者: 韩南银
  • 基金资助:

    北京市科委重大项目(D151100003815002).

Determination of six anticoccidials in chicken using QuEChERS combined with ultra high liquid chromatography-high resolution mass spectrometry

MUHAREM Muhteber1, YAN Hua2, XU Shan2, FENG Nan3, HAO Jie3, ZHU Chenqi1, GUO Shuang1, ZHANG Zhaohui2, HAN Nanyin1   

  1. 1. School of Pharmaceutical Science, Peking University, Beijing 100191, China;
    2. Inspection and Quarantine Testing Center, Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China;
    3. Beijing Municipal Center for Food Safety Monitoring and Risk Assessment, Beijing 100041, China
  • Received:2015-06-10 Online:2015-11-08 Published:2012-05-30

PDF

182

被引次数

21

摘要：

建立了鸡肉中二硝托胺、尼卡巴嗪、地克珠利、妥曲珠利、莫能菌素及盐霉素6种抗球虫药物的超高效液相色谱-高分辨串联质谱多残留检测方法。经QuEChERS样品净化,首先使用含有1%(v/v)三氯乙酸的乙腈-水(3 : 7, v/v)溶液提取样品中的被测物,再加入氯化钠,使用50 mg/mL N-丙基乙二胺(PSA)+50 mg/mL中性氧化铝(Alumina-N)的混合分散固相萃取(dispersive solid phase extraction, DSPE)粉末净化提取,过0.22 μ m滤膜后以超高效液相色谱-高分辨串联质谱检测。选择Waters Acquity UPLC® BEH C8色谱柱(100 mm×2.1 mm, 1.7 μ m),以甲醇-5 mmol/L醋酸铵水溶液为流动相进行梯度洗脱。使用正、负离子同时扫描模式,基质外标法定量。研究表明,6种目标化合物的线性范围为:二硝托胺,1.0~30.0 μ g/L;尼卡巴嗪,0.2~6.0 μ g/L;地克珠利、妥曲珠利,2.0~60.0 μ g/L;莫能菌素、盐霉素,4.0~120.0 μ g/L。空白样品中添加低、中、高3个水平的混合标准溶液,回收率在67.7%~126.8%之间,相对标准偏差(RSD)≤10.4%。6种抗球虫药物的定量限分别为:二硝托胺,2.50 μ g/kg;尼卡巴嗪,0.50 μ g/kg;地克珠利、妥曲珠利,5.00 μ g/kg;莫能菌素、盐霉素,20.00 μ g/kg。该方法操作简便,灵敏度高,且能够满足日常检测要求。

关键词: QuEChERS, 超高效液相色谱-高分辨串联质谱, 鸡肉, 抗球虫药

Abstract:

An ultra high liquid chromatography-Q Exactive orbitrap mass spectrometry multi-residue method has been developed for the determination of six anticoccidials residues (dinitlmide, nicarbazin, diclazuril, toltrazuril, monensin and salinomycin) in chicken tissue. Sample preparation was based on QuEChERS method, using 1% (v/v) trichloroacetic acid/acetonitrile aqueous solution (3 : 7, v/v) as the extraction solvent and salting-out with sodium chloride followed by clean-up with 50 mg/mL primary secondary amine (PSA)+50 mg/mL neutral alumina (Alumina-N) dispersive solid phase extraction (DSPE). The separation of the compounds in liquid chromatography was carried out using a Waters Acquity UPLC® BEH C8 column (100 mm×2.1 mm, 1.7 μ m) with mobile phases consisting of methanol-5 mmol/L ammonium acetate aqueous solution in gradient elution. The Q Exactive orbitrap mass spectrometric detection was carried out with positive and negative electrospray ionization simultaneously. The results showed the linear ranges of the six target compounds were as follows: dinitolmide, 1.0-30.0 μ g/L; nicarbazin, 0.2-6.0 μ g/L; diclazuril and toltrazuril, 2.0-60.0 μ g/L; monensin and salinomycin, 4.0-120.0 μ g/L. The external standard method was used for quantification. The spiked recoveries at three levels for the six anticoccidials ranged from 67.7% to 126.8%. The relative standard deviations (RSDs) were ≤10.4%. The limits of quantification (LOQs) were as follows: dinitolmide, 2.50 μ g/kg; nicarbazin, 0.50 μ g/kg; diclazuril and toltrazuril, 5.00 μ g/kg; monensin and salinomycin, 20.00 μ g/kg. The developed method is easy of operation and of high sensitivity. It can meet the requirements of daily inspection.

Key words: anticoccidials, chicken, QuEChERS, ultra high liquid chromatography-high resolution mass spectrometry

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