HPLC法同时测定金蝉止痒颗粒中9个成分的含量  

Simultaneous determination of nine constituents in Jinchan Zhiyang granules by HPLC

作　　者：何艳 袁志鹰[2] 夏新斌[2] HE Yan;YUAN Zhi-ying;XIA Xin-bin(College of Pharmacy,Xiang Nan University,Chenzhou 423000,China;Hunan University of Chinese Medicine,Changsha 410208,China)

机构地区：[1]湘南学院药学院,郴州423000 [2]湖南中医药大学,长沙410208

出　　处：《药物分析杂志》2022年第8期1363-1370,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：湖南省教育厅科学研究优秀青年项目(20B543);湖南省高新技术产业科技创新引领项目(科技攻关类)(2020SK2022);湖南省“十三五”药学应用特色学科基金(湘教通[2018]469号)。

摘　　要：目的:建立高效液相色谱(HPLC)同时测定金蝉止痒颗粒中栀子苷、连翘酯苷A、异绿原酸B、异绿原酸A、异绿原酸C、黄芩苷、盐酸小檗碱、汉黄芩苷和黄芩素含量的方法。方法:该样品采用70%甲醇水超声(功率500 W,频率40 kHz)提取,分析采用Waters Atlantis T3-C色谱柱(250 mm×4.6 mm, 5μm),流动相为乙腈-0.1%磷酸(含0.01 mol·L磷酸二氢钾),梯度洗脱,流速为1.0 mL·min,检测波长为240 nm(检测栀子苷)、328 nm(检测连翘酯苷A、异绿原酸B、异绿原酸A和异绿原酸C)、270 nm(检测黄芩苷、盐酸小檗碱、汉黄芩苷和黄芩素),柱温为30℃,进样量为10μL。结果:栀子苷、连翘酯苷A、异绿原酸B、异绿原酸A、异绿原酸C、黄芩苷、盐酸小檗碱、汉黄芩苷和黄芩素9个成分的线性范围和相关系数分别为2.330~23.30μg·mL(r=0.999 8)、2.494~24.94μg·mL(r=0.999 9)、1.064~10.64μg·mL(r=0.999 7)、0.905 1~9.051μg·mL(r=0.999 7)、1.038~10.38μg·mL(r=0.999 8)、6.792~67.92μg·mL(r=0.999 9)、5.822~58.22μg·mL(r=0.999 7)、1.193~11.93μg·mL(r=0.999 5)和0.561 6~5.616μg·mL(r=0.999 8),平均回收率(n=6)分别为96.9%(RSD=0.83%)、98.6%(RSD=1.3%)、101.6%(RSD=2.8%)、103.2%(RSD=2.6%)、103.6%(RSD=2.7%)、102.8%(RSD=1.1%)、98.2%(RSD=2.0%)、101.6%(RSD=1.8%)和98.8%(RSD=2.4%)。6批样品中上述9个成分含量范围依次分别为0.601 7~0.880 2、0.272 3~0.480 0、0.144 5~0.223 5、0.055 49~0.093 53、0.121 4~0.191 3、 0.638 2~1.697、0.930 9~1.657、0.171 7~0.359 8、0.029 65~0.089 54 mg·g。结论:本方法操作简便,重复性好,可用于金蝉止痒颗粒的质量控制。Objective: To establish a HPLC method for simultaneous determination of geniposide, forsythiaside A, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, baicalin, berberine hydrochloride, wogonoside and baicalein in Jinchan Zhiyang granules. Methods: The samples were extracted with 70% ethanol solution under ultrasonic(ultrasonic power, 500 W;ultrasonic frequency, 40 kHz) condition. The analysis was performed on a Waters Atlantis T3-Ccolumn(250 mm×4.6 mm, 5 μm) by gradient elution of acetonitrile-0.1% phosphoric acid solution(containing 0.01 mol·Lsolution of potassium dihydrogen phosphate) at a flow rate of 1.0 mL·min. The detection wavelengths were set at 240 nm(detecting geniposide), 328 nm(detecting forsythiaside A, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C) and 270 nm(baicalin, berberine hydrochloride, wogonoside and baicalein), the column temperature was 30 ℃, and the injection volume was 10 μL. Results: The linear ranges of geniposide, forsythiaside A, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, baicalin, berberine hydrochloride, wogonoside and baicalein were 2.330-23.30 μg·mL(r=0.999 8), 2.494-24.94 μg·mL(r=0.999 9), 1.064-10.64 μg·mL(r=0.999 7), 0.905 1-9.051 μg·mL(r=0.999 7), 1.038-10.38 μg·mL(r=0.999 8), 6.792-67.92 μg·mL(r=0.999 9), 5.822-58.22 μg·mL(r=0.999 7), 1.193-11.93 μg·mL(r=0.999 5) and 0.561 6-5.616 μg·mL(r=0.999 8), respectively. The average recoveries(n=6) were 96.9%(RSD=0.83%), 98.6%(RSD=1.3%), 101.6%(RSD=2.8%), 103.2%(RSD=2.6%), 103.6%(RSD=2.7%), 102.8%(RSD=1.1%), 98.2%(RSD=2.0%), 101.6%(RSD=1.8%), and 98.8%(RSD=2.4%), respectively. The content ranges of nine constituents in six batches of samples were 0.601 7-0.880 2 mg·gfor geniposide, 0.272 3-0.480 0 mg·gfor forsythiaside A, 0.144 5-0.223 5 mg·gfor isochlorogenic acid B, 0.055 49-0.093 53 mg·gfor isochlorogenic acid A, 0.121 4-0.191 3 mg·gfor isochlorogenic acid C, 0.638 2-1.697 mg·gfor baicalin, 0.930 9-1.657 mg·gfor berberine hydroch

关 键 词：金蝉止痒颗粒 高效液相色谱法 化学成分 栀子苷 连翘酯苷 异绿原酸 黄芩苷 盐酸小檗碱 汉黄芩苷 黄芩素 含量测定 质量控制 

分 类 号：R917[医药卫生—药物分析学]