目的：建立 HPLC 法同时测定气管炎丸中绿原酸、芍药苷、柚皮苷、黄芩苷、黄芩素、汉黄芩素的含 量。方法：采用 Agilent 5 TC -C18（2）（250 mm×4.6 mm,5 μm）色谱柱,以乙腈（A）-0.2%磷酸水溶液（B）为 流动 相,梯 度洗 脱（0~50 min,2%A → 34%A;50~61 min,34%A → 55%A;61~62 min,55%A → 2%A; 62~66 min,2%A）,流速 1.0 mL·min-1,柱温 30 ℃,检测波长分别为 327 nm（绿原酸）、230 nm（芍药苷）和280 nm（柚皮苷、黄芩苷、黄芩素、汉黄芩素）,进样体积 10 μL。结果：6 个活性成分在相应浓度范围内线性关系良好（r>0.999）;绿原酸、芍药苷、柚皮苷、黄芩苷、黄芩素、汉黄芩素的平均回收率分别为 101.0%（RSD=1.3%）、99.2%（RSD=1.1%）、98.3%（RSD=1.4%）、99.9%（RSD=1.3%）、101.2%（RSD=1.3%）、101.5%（RSD=1.3%）;精密度、稳定性、重复性良好,RSD 均小于 2%。含量测定结果分别为 0.295 9~0.375 8、 0.711 4~0.818 4、0.361 4~0.489 2、1.169~1.555、0.035 76~0.052 87、0.102 1~0.167 5 mg·g-1。结论：该方法简单、准确、快速,可为气管炎丸后续质量标准的提高提供实验参考。
Objective：To establish a method for the simultaneous determination of chlorogenic acid, paeoniflorin, naringin, baicalin, baicalein and wogonin in Qiguanyan pills. Methods：HPLC analysis was performed on the column of Agilent 5 TC-C18（2）（250 mm×4.6 mm, 5 μm）with the mobile phase of acetonitrile-0.2% phosphoric acid at a flow rate of 1.0 mL·min-1, the column temperature was 30 ℃, and the detection wavelength was 327 nm for chlorogenic acid, 230 nm for paeoniflorin and 280 nm for naringin, baicalin, baicalein, wogonin, and the volume injection was 10 μL. Results：Six active components showed good linear relationships within their own ranges（r>0.999）, the average recoveries were 101.0%（RSD=1.3%）, 99.2%（RSD=1.1%）, 98.3%（RSD=1.4%）, 99.9%（RSD=1.3%）, 101.2%（RSD=1.3%）and 101.5%（RSD=1.3%）respectively. The precision, stability, and repeatability were good with RSDs less than 2%. The content determination results of chlorogenic acid, paeoniflorin, naringin, baicalin, baicalein and wogonin were 0.295 9-0.375 8, 0.711 4-0.818 4, 0.361 4-0.489 2, 1.169-1.555, 0.035 76-0.052 87, 0.102 1-0.167 5 mg·g-1, respectively. Conclusion：The established method is simple, rapid, accurate and can be used for improvement of subsequent quality standards of Qiguanyan pills.
[1] 张生杰,王丽,田志梅.HPLC 波长切换法同时测定脑心通胶囊中 7 种指标成分[J].中国药科大学学报,2019,50(5):572
ZHANG SJ,WANG L,TIAN ZM.Simultaneous determination of seven index components in Naoxintong capsule by HPLC wavelength switching method[J].J China Pharm Univ,2019,50(5): 572
[2] 林雀跃,罗永强.张荣林,等.HPLC 法同时测定壮药玉叶金花中9 个成分的含量[J].药物分析杂志,2018,38(5):765
LIN QY,LUO YQ,ZHANG RL,et al.Simultaneous determination of nine components in Zhuang medicine Mussaenda pubescens Ait.f. by HPLC[J].Chin J Pharm Anal,2018,38(5):765
[3] 宋兴发,周军,郭守城.杏仁止咳合剂 HPLC 指纹图谱及 7 种成分的含量测定[J].中国现代应用药学,2020,37(1):50
SONG XF,ZHOU J,GUO SC.Study on HPLC fingerprints and content determination of 7 components in Xingren Zhike mixture[J].Chin J Mod Appl Pharm,2020,37(1):50
[4] 雷琪,田蜜.HPLC 法同时测定荨麻疹丸中 3 种有效成分的含量[J].中国药房,2016,27(24):3437
LEI Q,TIAN M.Simultaneous determination of three components in Urticaria pills by HPLC[J].China Pharm,2016,27(24):3437
[5] 陈辉,张石楠,马昕.双波长高效液相色谱法同时测定蓝芩口服液中 5 种化学成分的含量[J].中南药学,2018,26(10):1430
CHEN H,ZHANG SN,MA X.Simultaneous determination of 5 components in Lanqin oral solution by dual-wavelength HPLC[J]. Central South Pharm,2018,16(10):1430
[6] 武琳,杨光,黄菲.气管炎丸的质量标准研究[J].首都食品与医药,2015(6):51
WU L,YANG G,HUANG F.Study on quality standard for Qiguanyan pills[J].Cap Food Med,2015(6):51
[7] 邓永强,聂春发,施瑛,等.气管炎丸质量标准研究[J].医药导报,2013(10):1352
DENG YQ,NIE CF,SHI Y,et al.Study on quality control of Qiguanyan pills[J].Herald Med,2013(10):1352
[8] 李欣妍,邹桂欣,尤献民,等.气管炎丸中野鸢尾黄素含量测定[J].辽宁中医杂志,2016,43(7):1450
LI XY,ZOU GX,YOU XM,et al.Content determination of irigenin in compound Qiguanyan pills[J].Liaoning J Tradit Chin Med, 2016,43(7):1450
[9] 王莉萍,官炜,邓小晨.HPLC 法同时测定龙胆泻肝丸中 10 个成分的含量[J].中药材,2018,41(8):1923
WANG LP,GUAN W,DENG XC.Simultaneous determination of 10 componends in Longdan Xiegan pills by HPLC[J].J Chin Med Mater,2018,41(8):1923
[10] 李永生,张春玲,蒋凯.高效液相色谱法同时测定地榆炭中 8 种成分的含量[J].中南药学,2019,17(12):2154
LI YS,ZHANG CL,JIANG K.Simultaneous determination of 8 componends in carbonized sanguisorba root by HPLC[J].Central South Pharm,2019,17(12):2154
[11] 张威. 秦岭地区北柴胡遗传多样性及其质量评价研究[D].安徽:安徽中医药大学,2019
ZHANG W.Genetic Diversity and Quality Evaluation of Bupleurum chinense in Qinling mountains[D].Anhui:Anhui University of Chinese Medicine,2019
[12] 中华人民共和国药典2015 年版.一部[S].2015:74,105,301,332,352
ChP2015.Vol Ⅰ[S].2015:74,105,301,332,352
[13] 陈繁华,曾玉梅.对《中国药典》麻黄含量测定方法的改进[J]. 今日药学,2016,26(2):110
CHEN FH,ZENG YM.Improvement of determination method of ephedra content in Chinese Pharmacopoeia[J].Pharm Today,2016,26(2):110
[14] 蒋健. HPLC 法同时测定风寒感冒颗粒中苦杏仁苷、葛根素和橙皮苷的含量[J].中国药品标准,2019,20(6):482
JIANG J.Simultaneous determination of amygdalin,puerarin and hesperidin in Fenghan Ganmao granules by HPLC[J].Drug Stand China,2019,20(6):482
[15] 夏琴,张新选.HPLC 法测定蒲公英中绿原酸和咖啡酸的含量[J].西北药学杂志,2019,34(4):462
XIA Q,ZHANG XY.Determination of chlorogenic acid and caffeic acid in Taraxacum Herba by HPLC[J].Northwest Pharm J,2019, 34(4):462
[16] 高瑞苑,张艳,张海容.响应面法优化款冬花绿原酸的微波提取工艺[J].精细化工,2017,34(11):1246
GAO RY,ZHANG Y,ZHANG HR.Optimization of microwave extraction of chlorogenic acid from Tussilago Farfara by response surface methodology[J].Fine Chem,2017,34(11):1246
[17] 谢苗苗,刘婷婷,刘静,等.黄芩药材指纹图谱及其黄芩苷、黄芩素、汉黄芩素含量随地区分布差异的聚类分析[J].中医药导报,2019,25(7):45
XIE MM,LIU TT,LIU J,et al.The fingerprint of Huangqin (Scutellaria baicalensis) and the cluster analysis of the contents of baicalin,baicalein and hanbaicalein in Huangqin (Scutellaria baicalensis) with regional distribution differences[J].Guid J Tradit Chin Med Pharm,2019,25(7):45
