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0.22μm滤膜后以超高效液相色谱-高分辨串联质谱检测。选择Waters Acquity UPLCBEH C8色谱柱（100 mm×2.1 mm,1.7μm）,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,1.0~30.0μg/L;尼卡巴嗪,0.2~6.0μg/L;地克珠利、妥曲珠利,2.0~60.0μg/L;莫能菌素、盐霉素,4.0~120.0μg/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,2.50μg/kg;尼卡巴嗪,0.50μg/kg;地克珠利、妥曲珠利,5.00μg/kg;莫能菌素、盐霉素,20.00μg/kg。该方法操作简便,灵敏度高,且能够满足日常检测要求。
An ultra high liquid chromatography-Q Exactive orbitrap mass spectrometry multiresidue 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 UPLCBEH C8column（100 mm × 2. 1 mm,1. 7 μm）with mobile phases consisting of methanol-5 mmol / L ammonium acetate aqueous solution in gradient elution. The Q Exactive orbitrap massspectrometric 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 μg / L;nicarbazin,0. 2- 6. 0 μg / L;diclazuril and toltrazuril,2. 0- 60. 0μg / L;monensin and salinomycin,4. 0-120. 0 μg / L. The external standard method was used for quantification. The spiked recoveries at three levels for the six anticoccidials ranged from67. 7% to 126. 8%. The relative standard deviations（RSDs）were ≤10. 4%. The limits of quantification（LOQs）were as follows：dinitolmide,2. 50 μg / kg;nicarbazin,0. 50 μg / kg;diclazuril and toltrazuril,5. 00 μg / kg;monensin and salinomycin,20. 00 μg / kg. The developed method is easy of operation and of high sensitivity. It can meet the requirements of daily inspection.
出处
《色谱》
CAS
CSCD
北大核心
2015年第11期1199-1204,共6页
Chinese Journal of Chromatography
基金
北京市科委重大项目(D151100003815002)
