Determination of Cyproheptadine Hydrochloride in Swine Urine by Dispersive Liquid-Liquid Microextraction/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
  
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DOI:10.3969/j.issn.1004-4957.年份.月份
KeyWord:cyproheptadine hydrochloride  diphenylpyraline hydrochloride  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  internal standard method  dispersive liquid-liquid micro extraction(DLLME)
  
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吴剑平,张鑫,顾欣,李丹妮,严凤,周悦榕 上海市兽药饲料检测所
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Abstract:
      In order to determine the residue of cyproheptadine hydrochloride(CYP)in swine urine,an internal standard method,namely dispersive liquid-liquid micro extraction/ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method,was established.5 mL swine urine was adjusted to pH 11.0 by 5% aquous ammonia.The sample was extracted with 2 mL chloroform(extractant)-isopropyl alcohol(dispersant)by a ratio of 5∶3.The extractant was separated by 8 000 r/min centrifugation in 4 ℃,and evaporated with nitrogen at 50 ℃.The residue was dissolved with 1 mL 0.1% formic acid∶acenitril(80∶20)and detected by UPLC-MS using diphenylpyraline hydrochloride as an internal standard,with positive electrospray ionization under multi-reaction monitoring mode.The results showed that the linear range of CYP was in the range of 0.5-25 μg/L with a correlation coefficient of 0.999 5.The LOD of the method was 0.05 μg/L,while the LOQ was 0.1 μg/L.The recoveries of cyproheptadine hydrochloride at spiked range of 0.1-5.0 μg/L were in the range of 90.2%-109.7% with RSDs no more than 8.5%.The method showed good accuracy and precision.
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