【摘要】 [目的]采用分散固相萃取的前处理技术,建立了一种UPLC-MS/MS（ultra performance liquid chromatography-tandem mass spectrometry）法同时测定梅花鹿鹿鞭中18种磺胺的检测方法。[方法]鹿鞭样品以乙腈为提取剂,100 mg PSA、150 mg C₁₈与50 mg中性氧化铝为净化剂。液相色谱条件:ACQUITY BEH C₁₈柱（2.1 mm×100 mm,1.7μm）,流动相A为25 mmol/L甲酸乙腈,B为水,柱温35℃;质谱条件:正离子模式（ESI⁺）,多反应监测（multiple reaction monitoring,MRM）模式。鹿鞭中磺胺含量采用外标法定量。[结果]18种磺胺在0.05～50.00 ng/mL线性关系良好,决定系数R²均大于0.999,18种磺胺的检出限（LOD）为0.05μg/kg,定量限（LOQ）为0.15μg/kg。18种磺胺的平均加样回收率为83.5%～97.7%,RSD均小于5%。[结论]该方法具有操作简便、净化效果显著、灵敏度高、准确性好、检出限低等优点,可用于梅花鹿鹿鞭中18种磺胺的检测。更多还原

【Abstract】 [Objective]A method for the simultaneous determination of 18 sulfonamides in deer whip of Cervus nippon Temminck by UPLC-MS/MS was developed by using the pretreatment technology of dispersed solid phase extraction. [Method]Deer whip samples were extracted with acetonitrile and purified with 100 mg PSA, 150 mg C₁₈ and 50 mg neutral alumina. The UPLC analysis was carried out by a 35 ℃ thermostatic Waters Acquity UPLC BEH C₁₈ column（2.1 mm×100 mm,1.7 μm）with a mobile phase composed of 25 mmol/L formic acid acetonitrile-water for gradient elution at 0.3 mL/min. The detection was carried out on MS/MS with ESI in positive ion in the multiple reaction monitoring mode.The content of sulfonamides in pilose deer whip was quantified by external standard method.[Result] 18 kinds of sulfonamides had a good linear relationship between 0.05-50.00 ng/mL, the determination coefficient R2 were all greater than 0.999, LOD of 18 kinds of sulfonamides was 0.05 μg/kg, LOQ was 0.15 μg/kg. The average recovery of 18 sulfonamides was 83.5%-97.7%,RSD was less than 5%. [Conclusion]The method has the advantages of simple operation, remarkable purification effect, high sensitivity, good accuracy and low detection limit. It can be used for the determination of 18 sulfonamides in deer whip of Cervus nippon Temminck.更多还原