Muharem Muhteber, Yan Hua, Xu Shan, Feng Nan, Hao Jie, Zhu Chenqi, Guo Shuang, Zhang Zhaohui, Han Nanyin
Se Pu. 2015 Nov;33(11):1199-204. doi: 10.3724/sp.j.1123.2015.06016.
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 x 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 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 μg/L; nicarbazin, 0.2-6.0 μg/L; diclazuril and toltrazuril, 2.0-60.0 [μg/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 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 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.
建立了一种超高效液相色谱 - Q Exactive轨道阱质谱多残留方法，用于测定鸡肉组织中六种抗球虫药残留（二硝托胺、尼卡巴嗪、地克珠利、托曲珠利、莫能菌素和盐霉素）。样品制备基于QuEChERS方法，使用1%（v/v）三氯乙酸/乙腈水溶液（3:7，v/v）作为提取溶剂，用氯化钠盐析，然后用50 mg/mL的伯仲胺（PSA）+50 mg/mL中性氧化铝（Alumina - N）分散固相萃取（DSPE）进行净化。液相色谱中化合物的分离使用Waters Acquity UPLC BEH C8柱（100 mm×2.1 mm，1.7 μm），流动相由甲醇 - 5 mmol/L乙酸铵水溶液组成，进行梯度洗脱。Q Exactive轨道阱质谱检测同时采用正、负离子电喷雾电离。结果表明，六种目标化合物的线性范围如下：二硝托胺，1.0 - 30.0 μg/L；尼卡巴嗪，0.2 - 6.0 μg/L；地克珠利和托曲珠利，2.0 - 60.0 μg/L；莫能菌素和盐霉素，4.0 - 120.0 μg/L。采用外标法进行定量。六种抗球虫药在三个加标水平下的回收率为67.7%至126.8%。相对标准偏差（RSDs）≤10.4%。定量限（LOQs）如下：二硝托胺，2.50 μg/kg；尼卡巴嗪，0.50 μg/kg；地克珠利和托曲珠利，5.00 μg/kg；莫能菌素和盐霉素，20.00 μg/kg。所建立的方法操作简便、灵敏度高，能够满足日常检测的要求。
