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-C18 column (250 mm×4.6 mm, 5 μm) by gradient elution of acetonitrile-0.1% phosphoric acid solution (containing 0.01 mol·L-1 solution of potassium dihydrogen phosphate) at a flow rate of 1.0 mL·min-1. 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-1 (r=0.999 8), 2.494-24.94 μg·mL-1 (r=0.999 9), 1.064-10.64 μg·mL-1 (r=0.999 7), 0.905 1-9.051 μg·mL-1 (r=0.999 7), 1.038-10.38 μg·mL-1 (r=0.999 8), 6.792-67.92 μg·mL-1 (r=0.999 9), 5.822-58.22 μg·mL-1 (r=0.999 7), 1.193-11.93 μg·mL-1 (r=0.999 5) and 0.561 6-5.616 μg·mL-1 (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·g-1 for geniposide, 0.272 3-0.480 0 mg·g-1 for forsythiaside A, 0.144 5-0.223 5 mg·g-1 for isochlorogenic acid B, 0.055 49-0.093 53 mg·g-1 for isochlorogenic acid A, 0.121 4-0.191 3 mg·g-1 for isochlorogenic acid C, 0.638 2-1.697 mg·g-1 for baicalin, 0.930 9-1.657 mg·g-1 for berberine hydrochloride, 0.171 7-0.359 8 mg·g-1 for wogonoside and 0.029 65-0.089 54 mg·g-1 for baicalein. Conclusion: The established method is simple, reproducible, and can be used for the quality control of Jinchan Zhiyang granules.
[1] 贾琳, 江龙. 金蝉止痒颗粒质量标准分析与研究[J]. 中国医药导报, 2017, 14(22): 42
JIA L, JIANG L. Quality standard analysis and research for Jinchanzhiyang granules[J].Chin Med Her, 2017, 14(22): 42
[2] 陈琴华, 李鹏, 朱军, 等. 反相高效液相色谱法测定金蝉止痒颗粒中蛇床子素的含量[J].山西医药杂志, 2011, 40(6): 610
CHEN QH, LI P, ZHU J, et al. Determination of osthole in Jinchan Zhiyang granules by HPLC[J].Shanxi Med J, 2011, 40(6): 610
[3] 董文敏, 安叡, 宋舒雨, 等. 软坚清脉颗粒中5种主要成分的含量测定[J].中药新药与临床药理, 2021, 32(10): 1519
DONG WM, AN R, SONG SY, et al. Determination of five main components in Ruanjian Qingmai granules[J].Tradit Chin Drug Res Clin Pharm, 2021, 32(10): 1519
[4] 宋京美, 龚韬, 杨薇,等. HPLC测定益肾骨康颗粒中莫诺苷、马钱苷、野黄芩苷、柚皮苷的含量[J].中国现代应用药学, 2021, 38(7): 841
SONG JM, GONG T, YANG W, et al. Determination of morroniside, loganin, scutellarin and naringin in Yishen Gukang granules by HPLC[J].Chin J Mod Appl Pharm, 2021, 38(7): 841
[5] 王玉林, 邵晓玮, 王建强, 等. HPLC法同时测定万氏牛黄清心丸中7种成分[J].中成药, 2021, 43(3): 601
WANG YL, SHAO XW, WANG JQ, et al. Simultaneous determination of seven constituents in Wan's Niuhuang Qingxin pills by HPLC[J].Chin Tradit Pat Med, 2021, 43(3): 601
[6] 林永强, 林林, 焦阳, 等. 基于Q-Marker理论的化学标识物研究及应用[J].中国药学杂志,2020, 55(2): 161
LIN YQ, LIN L, JIAO Y, et al. Research and application of chemical marker based on Q-marker theory[J].Chin Pharm J, 2020, 55(2): 161
[7] 何艳, 胡小祥, 王庆. HPLC法同时测定感冒止咳颗粒中10种成分[J].中成药, 2020, 42(4): 849
HE Y, HU XX, WANG Q. Simultaneous determination of ten constituents in Ganmao Zhike granules by HPLC[J].Chin Tradit Pat Med, 2020, 42(4): 849
[8] 胡杨, 李先芝, 钱全全, 等. HPLC法同时测定金银花配方颗粒中6种成分[J].中成药, 2021, 43(7): 1717
HU Y, LI XZ, QIAN QQ, et al. Simultaneous determination of six consituents in Jinyinhua formula granules by HPLC[J].Chin Tradit Pat Med, 2021, 43(7): 1717
[9] 缪艳燕, 徐帮会, 徐剑, 等. 金银花的HPLC指纹图谱建立及其抗炎作用谱-效关系研究[J].中国药房, 2020, 31(20): 2497
MIAO YY, XU BH, XU J, et al. Establishment of HPLC fingerprint of Lonicera japonica and study on its anti-inflammatory spectrumeffect relationship[J].China Pharm, 2020, 31(20): 2497
[10] 王越欣, 苗雨露, 王梅, 等. 青翘和老翘的HPLC指纹图谱比较及聚类分析、主成分分析[J].中国药房, 2021, 32(6): 663
WANG YX, MIAO YL, WANG M, et al. Comparison of HPLC fingerprint, cluster analysis and principle component analysis of green Forsythia suspensa and grown F. suspensa[J].China Pharm, 2021, 32(6): 663
[11] 朱鹤云, 王开鼎, 史健艺, 等. UFLC-MS/MS法同时测定栀子厚朴汤中10个成分的含量[J].药物分析杂志, 2020, 40(10): 1751
ZHU HY, WANG KD, SHI JY, et al. Simultaneous determination of ten components in Zhizi Houpo decoction by UFLC-MS/MS[J].Chin J Pharm Anal, 2020, 40(10): 1751
[12] 彭平, 熊少哲, 张蓓, 等. 基于全方特征图谱质量表征的芩连制剂质量评价研究[J].中草药,2021, 52(5): 1312
PENG P, XIONG SZ, ZHANG B, et al. Quality evaluation of Qinlian preparations based on quality characterization of whole prescription characteristic spectrum[J].Chin Tradit Herb Drugs, 2021, 52(5): 1312
[13] 王宇卿, 李淑娇. 基于HPLC-ABTS-DAD-Q-TOF/MS的黄芩抗氧化活性成分研究[J].中草药,2019, 50(3): 568
WANG YQ, LI SJ. Anti-oxidant components in Scutellaria baicalensis based on HPLC-ABTS-DAD-Q- TOF/MS[J].Chin Tradit Herb Drugs, 2019, 50(3): 568
[14] 陈韶彬, 曹玲, 张莉, 等. 功劳去火胶囊中多种指标性成分的同时测定[J].药物分析杂志,2020, 40(11): 1994
CHEN SB, CAO L, ZHANG L, et al. Simultaneous determination of index components in Gonglao Quhuo capsules[J].Chin J Pharm Anal, 2020, 40(11): 1994
[15] 王福成, 李冬华, 郭文宾, 等. HPLC-DAD法同时测定栀子金花丸中10个成分的含量[J].药物分析杂志, 2020, 40(1): 145
WANG FC, LI DH, GUO WB, et al. Simultaneous determination of ten components in Zhizi Jinhua pills by HPLC-DAD[J].Chin J Pharm Anal, 2020, 40(1): 145
[16] 吴晶, 刘鸿雁, 于博, 等. HPLC波长切换法同时测定苍柏祛痛胶囊中的6种成分[J].华西药学杂志, 2019, 34(2): 165
WU J, LIU HY, YU B, et al. Simultaneous determination of six constituents in Cangbai qutong capsules by HPLC wavelength switching[J].West China J Pharm Sci, 2019, 34(2): 165
