摘要
目的:建立同时测定黄连-吴茱萸药对中4种有效成分含量的方法,探讨该药对的合理比例。方法:采用高效液相色谱法。色谱柱为Welch XB C_(18),流动相为乙睛-1.5 mmol/L十二烷基硫酸钠溶液(磷酸调p H至5.0)(梯度洗脱),流速为1.0 mL/min,检测波长为265 nm,柱温为30℃,进样量为10μL。结果:盐酸小檗碱、盐酸巴马汀、吴茱萸碱、吴茱萸次碱检测质量浓度线性范围分别为2.24~44.80μg/m L(r=0.999 9)、1.26~31.50μg/mL(r=0.999 8)、2.70~81.00μg/mL(r=0.999 8)、1.65~49.50μg/mL(r=0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为98.11%~100.73%(RSD=1.04%,n=6)、96.54%~103.47%(RSD=1.86%,n=6)、95.49%~102.36%(RSD=2.05%,n=6)、97.19%~103.24%(RSD=2.19%,n=6)。当黄连-吴茱萸比例(m/m)为2∶1时,各成分综合含量最高。结论:该方法操作简便,精密度、稳定性、重复性好,可用于不同配伍比例黄连-吴茱萸药对中4种有效成分含量的同时测定;该药对中黄连-吴茱萸比例(m/m)为2∶1较合理。
OBJECTIVE: To establish a method for simultaneous determination of 4 effective components in the couple of Cop- tidis Rhizoma and Evodiae Fructus, and to investigate rational proportion of the couple. METHODS : HPLC method was adopted. The determination was performed on Welch XB C18 column with mobile phase consisted of acetonitrile-l.5 mmol/L sodium dodecyl sulfate solution (pH adjusted to 5.0 with phosphoric acid) (gradient elution) at the flow rate of 1.0 mL/min. The detection wave- length was set at 265 nm, and the column temperature was 30℃. The sample size was 10 μL. RESULTS: The linear ranges of ber- berine hydrochloride, martin hydrochloride, evodiamine and rutacarpine were 2.24-44.80 μg/mL(r=0.999 9), 1.26-31.50 μg/mL (r=0.999 8), 2.70-81.00 μg/mL(r=0.999 8), 1.65-49.50 pg mL(r=0.999 9), respectively. RSDs of precision, stability and re- producibility tests were all lower than 3.0 %. The recoveries were 98.11%-100.73 % (RSD = 1.04%, n = 6 ), 96.54 %- 103.47 % (RSD = 1.86%, n=6), 95.49%-102.36% (RSD=2.05%, n=6), 97.19%-103.24% (RSD=2.19%, n=6), respectively. When the propor- tion of Coptidis Rhizoma-Evodiae Fructus (m/m) was 2: 1, the comprehensive content of each component was the highest. CON- CLUSIONS : The method is simple, accurate, stable and reproducible, and can be used for simultaneous determination of 4 effec- tive components in different compatibility proportions of the couple of Coptidis Rhizoma and Evodiae Fructus. The rational propor- tion of the couple of Coptidis Rhizoma and Evodiae Fructus is 2 : 1.
出处
《中国药房》
CAS
北大核心
2017年第24期3430-3432,共3页
China Pharmacy
关键词
黄连
吴茱萸
药对
高效液相色谱法
盐酸小檗碱
盐酸巴马汀
吴茱萸碱
吴茱萸次碱
含量测定
Coptidis Rhizoma
Evodiae Fructus
Couple
HPLC
Berberine hydrochloride
Martin hydrochloride
Evodia alka-loid
Rutacarpine
Content determination