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 UPLC? BEH 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 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 neu-tral 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 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 simul-taneously. 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 from 67. 7% to 126. 8%. The relative standard deviations( RSDs)were ≤10. 4%. The limits of quanti-fication( 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.
参考文献
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| [2] | Usui,K.;Hayashizaki,Y.;Minagawa,T.;Hashiyada,M.;Nakano,A.;Funayama,M..Rapid determination of disulfoton and its oxidative metabolites in human whole blood and urine using QuEChERS extraction and liquid chromatography-tandem mass spectrometry[J].Legal medicine,20126(6):309-316. |
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