摘要
目的:建立超高效液相色谱串联三重四级杆质谱法测定羚羊角中羚羊角肽的含量,为提高相关药品的质量控制水平提供参考。方法:采用色谱柱ACQUITY UPLC■BEH C18(2.1mm×50mm,1.7μm),流速0.3mL/min,梯度洗脱,电喷雾离子化(ESI),正离子模式下,多反应监测,鞘气流速46L/h;辅助气流速850L/h;喷雾电压3.5kV;离子源温度150℃;辅助气温度400℃;选择m/z(三电荷)697.66→1021.48为定量离子对。结果:羚羊角肽在0.02528~2.528μg/mL范围内,浓度与色谱峰面积成良好的线性关系,回归方程y=15309x+91.47(r=0.9996)。回收率在90.9%~106.2%范围内,平均回收率为100.9%,RSD值为5.2%。结论:建立的含量测定方法准确、可靠,不同羚羊角粉内在质量差异显著,该研究对相关药品的标准提高及质量控制具有很高的参考价值。
Objective:To establish a method for the determination of antelope horn peptide in antelope horn by UPLC MS/MS,and to provide reference for improving the quality control of related drugs.Methods:Chromatographic column ACQUITY UPLC■BEH C18(2.1 mm×50 mm,1.7μm)was used,and the flow rate was 0.3 mL/min with gradient elution.The electrospray ionization(ESI)and multiple reaction monitoring(MRM)were carried out under positive ion mode.The sheath gas flow rate was 46 L/h,auxiliary air flow speed was 850 L/h,spray voltage was 3.5 kV,the ion source temperature was 150℃,and auxiliary gas temperature was 400℃.The m/z(three charges)697.66→1021.48 was chosen as the quantitative ion pair.Results:The antelope horn peptide was in the range of 0.02528~2.528μg/mL.The concentration had a good linear relationship with the chromatographic peak area,and the regression equation was y=15309 x+91.47(r=0.9996).The recovery rate range was 90.9%~106.2%,the average recovery rate was 100.9% and the RSD was 5.2%.Conclusion:The established content determination method is accurate and reliable,and the inherent quality of different antelope horn powders is significantly different.This study has a high reference value for improving the standards and quality control of related drugs.
作者
王玉团
石峰
杭宝建
WANG Yu-tuan;SHI Feng;HANG Bao-jian(Shandong Institute for Food and Drug Control,Jinan 250101,China)
出处
《中华中医药杂志》
CAS
CSCD
北大核心
2020年第7期3698-3701,共4页
China Journal of Traditional Chinese Medicine and Pharmacy
关键词
羚羊角
羚羊角肽
含量
多肽
Antelope horn
Antelope horn peptide
Content
Polypeptide
