超高效液相色谱法测定牧草中马来酸麦角新碱含量

Determination of ergometrine maleate in herbage by ultra performance liquid chromatography

中文关键词:  马来酸麦角新碱  超高效液相色谱法  牧草

英文关键词:ergometrine maleate  ultra performance liquid chromatography  herbage

中文摘要:

      目的 建立超高效液相色谱法(ultra performance liquid chromatography, UPLC)测定牧草中马来酸麦角新碱含量的分析方法。方法 样品经纯甲醇提取后, 过混合阳离子(MCX)固相萃取柱净化。采用5 mmol/L乙酸铵溶液(含0.1%甲酸)(A)和乙腈(B)作为流动相进行梯度洗脱, 超高效液相色谱采用二极管阵列紫外检测器进行定量。结果 本方法的检测限为0.5 mg/kg, 定量限为2 mg/kg, 方法在0.05~5 μg/mL范围内线性良好(r=1), 在2、10和20 mg/kg添加水平的回收率为83.80%~94.49%, 相对标准偏差≤3.5% (n=5), 实际样品测定结果为6.3~194.8 mg/kg。结论 本方法具有良好的正确度和精密度, 能有效测定牧草中马来酸麦角新碱含量, 为将来马来酸麦角新碱应用到畜牧业打下了基础。

英文摘要:

      Objective To establish an analytical method for determining ergometrine maleate content in herbage by ultra performance liquid chromatography (UPLC). Methods The samples were extracted with pure methanol, and purified using a mixed cation (MCX) solid-phase extraction column. Gradient elution was performed using 5 mmol/L ammonium acetate solution containing 0.1% formic acid (A) and acetonitrile (B) as the mobile phases, and quantitation was performed on UPLC using a diode array UV detector. Results The detection limit and quantitation limit of the method were 0.5 mg/kg and 2 mg/kg, respectively. The linearity was good within the range of 0.05? 5 μg/mL (r=1). The recoveries were 83.80%?94.49% at the 2, 10, and 20 mg/kg levels. The relative standard deviation was less than 3.5% (n=5). The actual sample determination results were 6.3?194.8 mg/kg. Conclusion This method has good accuracy and precision, and can effectively determine the ergometrine maleate content in forage, which lays a foundation for the application of ergometrine maleate to animal husbandry in the future.