分散液相微萃取/超高效液相色谱-串联质谱法检测猪尿中盐酸赛庚啶残留量的研究

摘要

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 0.5-25μg/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.%建立了猪尿中盐酸赛庚啶残留量的分散液相徽萃取(DLLME)/超高效液相色谱-串联质谱内标检测法.将5 mL猪尿用5％氨水调节至pH 11.0,以三氯甲烷为萃取剂,异丙醇为分散剂,配比为5∶3,组成微萃取体系共2 mL进行分散液相微萃取,4℃下以8 000 r/min高速离心5min后获得提取液,在50℃下氮气吹干后,经1 mL0.1％甲酸-乙腈(80∶20)溶解后使用超高效液相色谱-三重四极杆串联质谱检测,以盐酸二苯拉林(Diphenylpyraline,DPP)为内标,正离子电喷雾下多反应监测模式进行分析.结果显示,标准品溶液在0.5～ 25 μg/L范围内线性关系良好(r=0.999 5),方法的检出限为0.05 μg/L,定量下限为0.1μg/L.尿样在0.1～5.0 μg/L加标范围内的回收率为90.2％～109.7％,RSD不高于8.5％,表明该方法具有较好的准确度与精密度.