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 hydrochloride, 0.171 7-0.359 8 mg·gfor wogonoside and 0.029 65-0.089 54 mg·gfor baicalein. Conclusion: The established method is simple, reproducible, and can be used for the quality control of Jinchan Zhiyang granules.
作者
何艳
袁志鹰
夏新斌
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)
出处
《药物分析杂志》
CAS
CSCD
北大核心
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)。
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
Jinchan Zhiyang granules
HPLC
chemical constituents
geniposide
forsythiaside
isochlorogenic acid
baicalin
berberine hydrochloride
wogonoside
baicalein
content determination
quality control
