HPLC法测定半贝丸中腺苷、鸟苷、西贝母碱和西贝母碱苷的含量  

Content Determination of Adenosine,Guanosine,Sipeimine and Sipeimine-3β-d-glucoside in Banbei Pill by HPLC

作　　者：许红莉[1] 邓新红 

机构地区：[1]孝感市康复医院,湖北孝感432000 [2]孝感市中医院,湖北孝感432000

出　　处：《中国药房》2014年第47期4478-4480,共3页China Pharmacy

摘　　要：目的：建立半贝丸中腺苷、鸟苷、西贝母碱和西贝母碱苷的含量测定方法。方法：采用高效液相色谱（HPLC）法。腺苷和鸟苷的色谱柱为Hypersil C18（250 mm×4.6 mm,5μm）,流速为0.9 ml/min,流动相为甲醇-1%冰醋酸（梯度洗脱）,检测波长为260nm;西贝母碱和西贝母碱苷的色谱柱为Hpersil C18（250 mm×4.6 mm,5μm）,流动相为乙腈-0.1%二乙胺溶液（79∶21,V/V）,柱温为室温,流速为0.9 ml/min,进样量为10μl,蒸发光散射检测器漂移管温度为85℃,载气（N2）流速为2.1 L/min。结果：腺苷与鸟苷的进样量分别在0.013 4～0.268 0μg（r=0.999 2）、0.041 2～0.824 0μg（r=0.999 7）范围内与峰面积积分值呈良好线性关系,平均加样回收率分别为97.66%、96.86%,RSD分别为1.72%、1.38%（n均为6）;西贝母碱和西贝母碱苷进样量分别在0.031 6～0.632 0（r=0.999 1）、0.065 2～1.304 0μg（r=0.999 8）范围内与各自峰面积的自然对数值呈良好线性关系,平均加样回收率分别为96.51%、98.79%,RSD分别为1.37%、0.94%（n均为6）。精密度、稳定性、重复性试验的RSD均小于1%。结论：该测定方法结果准确、灵敏度高、重复性好,可为完善半贝丸的质量控制标准提供依据。OBJECTIVE： To determine the contents of adenosine, guanosine, sipeimine and sipeimine-3β-d-glucoside in Ban- bei pill. METHODS：HPLC method was adopted. The determination was performed on Hypersil C18（250 mm×4.6 mm, 5 μm） col- umn at the flow rate of 0.9 ml/min. The mobile phase of adenosine and guanosine consisted of methanol-1% acetic acid at the detec- tion wavelength of 260 nm. The determination of sipeimine and sipeimine-3β-d-glucoside was performed on Hypersil C18 （250 mm× 4,6 mm, 5 μm）column with mobile phase consisted of acetonitrile-0.1% diethylamine solution （79：21, V/V）at the flow rate of 0.9 ml/min. The cloumn temperature was room temperture and sample size was 10 μl. The temperature of drift tube was set at 85 ℃, and N2 was used as carrier gas at the flow rate of 2.1 L/min. RESULTS： The linear range was 0.013 4-0.268 0 μg for adenosine（r= 0.999 2） and 0.041 2-0.824 0 p.g for guanosine（r=0.999 7）; average recoveries were 97.66% （RSD=1.72%, n=6） and 96.86% （RSD=1.38% ,n=6）. The linear range was 0.031 6-0.632 0 μg for sipeimine（r=0.999 1） and 0.065 2-1.304 0 μg for sipeimine-3 β-d-glucoside（r=0.999 8） ; average recoveries were 96.51% （RSD=1.37%, n=6） and 98.79% （RSD=0.94%, n=6）. RSDs of precision, stability and reproducibilsty tests were all louer than 1%. CONCLUSIONS： The method is accurate, sensitive and repro- ducible, and can provide reference for the improvement of quality control standard of Banbei pill.

关 键 词：半贝丸 腺苷 鸟苷 西贝母碱 西贝母碱苷 高效液相色谱法 

分 类 号：R927.2[医药卫生—药学]