摘要
目的:建立测定红卫蛇药片中薯蓣皂苷元、黄独乙素、鬼臼毒素和山柰素含量的方法。方法:采用高效液相色谱法。色谱柱为Hypersil C18,流速为1.0 ml/min;薯蓣皂苷元和黄独乙素的流动相为乙腈-水-磷酸(67∶33∶0.5,V/V/V),检测波长为305 nm;鬼臼毒素和山柰素的流动相为甲醇-乙腈-0.1 mol/L磷酸二氢钾水溶液(55∶40∶5,V/V/V),检测波长为360 nm。结果:薯蓣皂苷元和黄独乙素的进样量分别在0.109 4~2.188 0、0.328 6~6.572 0μg范围内与各自峰面积积分值呈良好线性关系(r=0.999 5、0.999 2);精密度、稳定性、重复性试验的RSD均〈1%;平均加样回收率分别为98.01%、97.14%,RSD分别为1.01%、0.79%(n=6)。鬼臼毒素和山柰素的进样量分别在0.159 8~3.196 0、0.033 4~0.668 0μg范围内与各自峰面积积分值呈良好线性关系(r=0.999 3、0.999 7);精密度、稳定性、重复性试验的RSD均〈1%;平均加样回收率分别为98.04%、96.87%,RSD分别为1.59%、1.19%(n=6)。结论:该方法操作简便、灵敏度高、重复性好,结果准确、可靠,可用于红卫蛇药片的质量控制。
OBJECTIVE: To develop a method for the content determination of diosgenin, diosbulbin B, podophyllotoxin and kaempferol in HWSYP. METHODS: HPLC method was adopted. The determination was performed on Hypersil C18 column at the flow rate of 1.0 ml/min. The mobile phase of diosgenin and diosbulbin B consisted of acetonitrile-water-phosphoric acid (67 : 33 : 0.5, V/V/V), and detection wavelength was set at 305 nm. That of podophyllotoxin and kaempferol consisted of methanol-acetonitrile-0.1 mol/L KI-IePO4(55 : 40: 5, V/V/V) , and detection wavelength was set at 360 nm. RESULTS: The linear range of diosgenin and diosbulbin B were 0.109 4-2.188 0 μg(r=0.999 5)and 0.328 6-6.572 0 μg(r=0.999 2); RSDs of precision, stability and reproducibility tests were all lower than 1%; average recoveries were 98.01% (RSD=1.01% ,n=6) and 97.14% (RSD=0.79% ,n=6). The linear range of podophyllotoxin and kaempferol were 0,159 8-3.196 0 μg(r=0.999 3)and 0.033 4-0.668 0 μg(r=0.999 7); RSDs of precision, stability and reproducibility tests were all lower than 1%; average recoveries were 98.04% (RSD= 1.59%, n=6) and 96.87% (RSD=1.19%, n=6). CONCLUSIONS: The method is simple, sensitive, accurate, reliable and reproducible, and can be used for the quality control of HWSYP.
出处
《中国药房》
CAS
北大核心
2015年第3期407-410,共4页
China Pharmacy