摘要
目的:建立超高效液相色谱-质谱法(UPLC-MS/MS)同时测定痔血合剂中没食子酸、芦丁、栀子苷、槲皮苷、阿魏酸、柚皮苷、新橙皮苷、黄芩苷8种成分的含量。方法:采用AcquityUPLCBEHC18色谱柱(2.1mm×50mm,1.7μm),流动相:甲醇-水(含2mmol·L^-1甲酸铵)(65∶35),流速:300μL·min^-1,柱温:35℃,进样量:2μL;质谱采用电喷雾离子化(ESI),负离子检测,多反应监测(MRM)模式。结果:没食子酸、芦丁、栀子苷、槲皮苷、阿魏酸、柚皮苷、新橙皮苷、黄芩苷的线性范围分别为7.813~250.0ng·mL^-1(r=0.9886)、62.50~2000ng·mL^-1(r=0.9934)、15.63~500.0ng·mL^-1(r=0.9755)、0.7813~25.00ng·mL^-1(r=0.9894)、0.7813~25.00ng·mL^-1(r=0.9996)、62.50~2000ng·mL^-1(r=0.9939)、62.50~2000ng·mL^-1(r=0.9968)、15.63~500.0ng·mL^-1(r=0.9998)。精密度、重复性、稳定性试验的RSD均符合要求。没食子酸、芦丁、栀子苷、槲皮苷、阿魏酸、柚皮苷、新橙皮苷、黄芩苷的平均加样回收率分别为96.90%、97.98%、101.18%、98.00%、99.22%、98.60%、98.38%、99.00%。结论:本法灵敏简便、准确度高,可同时测定痔血合剂中8种成分的含量,为其质量控制提供参考。
Objective: An UPLC-MS/MS method was established to determine gallic acid, rutin, geniposide, quercitrin, ferulic acid, naringin, neohesperidin and baicalin in Zhixue Mixture. Methods: The determination was performed on an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) with mobile phase of methanol -water (containing 2 mmol·L^-1 ammonium formate)(65∶35) at the flow rate of 300 μL·min^-1. Electrospray ionization model (ESI) and multiple reaction monitoring (MRM) model were used for quantification. Results: The linear ranges of gallic acid, rutin, geniposide, quercitrin, ferulic acid, naringin, neohesperidin and baicalin were 7.813-250.0 ng·mL^-1 (r=0.988 6), 62.50-2 000 ng·mL^-1 (r=0.993 4), 15.63-500.0 ng·mL^-1 (r=0.975 5), 0.781 3-25.00 ng·mL^-1 (r=0.989 4), 0.781 3-25.00 ng·mL^-1 (r=0.999 6), 62.50-2 000 ng·mL^-1 (r=0.993 9), 62.50-2 000 ng·mL^-1 (r=0.996 8) and 15.63-500.0 ng·mL^-1 (r=0.999 8), respectively. Precision, reproducibility and stability RSD all met the requirements. The average recoveries of gallic acid, rutin, geniposide, quercitrin, ferulic acid, naringin, neohesperidin and baicalin were 96.90%, 97.98%, 101.18%, 98.00%, 99.22%, 98.60%, 98.38% and 99.00% respectively. Conclusions: The established method is proved to be sensitive, convenient, accurate and suitable for simultaneous determination of eight compounds in Zhixue Mixture.
作者
孙冰婷
赵颖
庞鹏
SUN Bingting;ZHAO Yin;PANG Peng(Department of Pharmacy,Nanjing Hospital of Traditional Chinese Medicine,Nanjing 210001)
出处
《药学与临床研究》
2019年第5期345-348,共4页
Pharmaceutical and Clinical Research
