Objective: To establish an LC-MS/MS method for simultaneous determination of 13 components (geniposide, albiflorin, paeoniflorin, forsythoside A, liquiritin, baicalin, forsythin, oroxylin A-7-O-β-D-glucuronide, wogonoside, baicalein, wogonin, rhein and glycyrrhizic acid) in Xiao’er Chiqiao Qingre granules. Methods: The separation was performed on a Poroshell 120 SB-C18 column(100 mm×3.0 mm, 2.7 μm) by gradient elution, with mobile phase consisting of 0.1% formic acid aqueous and methanol-acetonitrile(1∶1) at a flow rate of 0.45 mL·min-1and the column temperature of 40 ℃. The MS analysis was performed on a triple quadrupole mass spectrometer with an electrospray ionization(ESI) source operated in negative ion mode and multiple reaction monitoring(MRM). Results: The method had a good linearity in the ranges of 9-900 ng·mL-1 for geniposide, 1-100 ng·mL-1 for albiflorin, 12-1 200 ng·mL-1 for paeoniflorin, 12-1 800 ng·mL-1 for forsythoside A, 1-100 ng·mL-1 for liquiritin, 8-800 ng·mL-1 for baicalin, 5-500 ng·mL-1 for forsythin, 5-500 ng·mL-1 for oroxylin A-7-O-β-D-glucuronide, 5-500 ng·mL-1 for wogonoside, 2-200 ng·mL-1 for baicalein, 0.4-40 ng·mL-1 for wogonin, 0.4-40 ng·mL-1 for rhein and 5-500 ng·mL-1 for glycyrrhizic acid(r>0.998 5). The average recoveries(n=6) of them were 97.0%-110.5% with the RSDs of 3.2%-9.6%. The contents of 13 components in 5 batches of Xiao’er Chiqiao Qingre granules were 4.933-5.800 mg·g-1 of geniposide, 0.104-0.123 mg·g-1 of albiflorin, 3.140-4.159 mg·g-1 of paeoniflorin, 17.40-21.05 mg·g-1 of forsythoside A, 0.354-0.425 mg·g-1 of liquiritin, 4.991-6.422 mg·g-1 of baicalin, 1.446-1.906 mg·g-1 of forsythin, 0.441-0.534 mg·g-1 of oroxylin A-7-O-β-D-glucuronide, 0.925-1.138 mg·g-1 of wogonoside, 0.129-0.151 mg·g-1 of baicalein, 0.084-0.106 mg·g-1 of wogonin, 0.051-0.063 mg·g-1 of rhein and 0.964-1.242 mg·g-1 of glycyrrhizic acid. Conclusion: The method is specific, sensitive, effective and reliable, and can be used for quality control of Xiao’er Chiqiao Qingre granules.
[1] 中华人民共和国药典2020年版. 一部[S].2020:582
ChP 2020. VolⅠ[S].2020: 582
[2] 宋根伟, 王鑫, 金萍, 等. 小儿豉翘清热颗粒临床应用进展[J].中国药业, 2015, 24(2):91
SONG GW, WANG X, JIN P, et al. Progress in clinical application of Xiao’er Chiqiao Qingre granules[J].China Pharm, 2015, 24(2): 91
[3] 韩登高, 郭清, 巨慧, 等. 小儿豉翘清热颗粒治疗病毒性上呼吸道感染患儿发热(风热夹滞证)的效果观察[J].中药材, 2018,41(8):2013
HAN DG, GUO Q, JU H, et al. Observation of Xiao’er Chiqiao Qingre granules in the treatment of fever caused by viral upper respiratory tract infection (wind-heat clip hysteresis syndrome) in children[J].J Chin Med Mater, 2018, 41(8): 2013
[4] 曾娇, 胡德飞, 陈东长. 小儿病毒性上呼吸道感染采用小儿豉翘清热颗粒治疗疗效分析[J].当代医学, 2018,24(17): 141
ZENG J, HU DF, CHEN DC. Effect of Xiao’er Chiqiao Qingre granules on the fever caused by viral upper respiratory tract infection in children[J].Contemp Med, 2018, 24(17): 141
[5] 周晓萍. 小儿豉翘颗粒联合同笑口服液治疗小儿疱疹性咽峡炎的疗效探析[J].当代医药论丛, 2017,15(18): 26
ZHOU XP. Effect of Xiao’er Chiqiao Qingre granules combined with Tongxiao oral solution for treatment of pediatric herpangina[J].Contemp Med Symp, 2017, 15(18): 26
[6] 岳素文. 小儿豉翘清热颗粒治疗儿童疱疹性咽炎疗效观察[J].世界最新医学信息文摘, 2017, 17(95): 115
YUE SW. Effect of Xiao’er Chiqiao Qingre granules on pediatric herpangina[J].World Latest Med Inf, 2017, 17(95): 115
[7] 宋根伟, 金萍, 赵利军, 等. HPLC同时测定小儿豉翘清热颗粒中两种苷含量[J].湖北医药学院学报, 2015, 34(4): 344
SONG GW, JIN P, ZHAO LJ, et al. Simultaneous determination of the contents of geniposide and baicalin in Xiaoer Chiqiao Qingre granule by high performance liquid chromatography[J].J Hubei Univ Med, 2015, 34(4): 344
[8] 田刚, 李超, 吴菲, 等. 基于一测多评法对小儿豉翘清热颗粒中9个成分的质量控制[J].药物分析杂志, 2018,38(11): 1922
TIAN G, LI C, WU F, et al. Quality control of 9 components in Xiao’er Chiqiao Qingre granules by multi-components with a single-marker(QAMS)[J].Chin J Pharm Anal, 2018, 38(11): 1922
[9] 田刚, 杨学芳, 李超, 等. UPLC同时检测小儿豉翘清热颗粒中9种成分的含量[J].中国中药杂志, 2018,43(10): 2081
TIAN G, YANG XF, LI C, et al. Simultaneous determination of 9 components in Xiao’er Chiqiao Qingre granules by UPLC[J].China J Chin Mater Med, 2018, 43(10): 2081
[10] 周蓬, 宋青, 马帅. HPLC法同时测定小儿豉翘清热颗粒中栀子苷、芍药苷、黄芩苷、黄芩素和汉黄芩素[J].中成药, 2013, 35(8): 1693
ZHOU P, SONG Q, MA S. Simultaneous determination of geniposide, peoniflorin, baicalin, baicalein and wogonin in Xiao’er Chiqiao Qingre granules by HPLC[J].Chin Tradit Pat Med, 2013, 35(8): 1693
[11] 许文清, 魏学涛, 马青青, 等.小儿豉翘清热颗粒HPLC-PAD指纹图谱的建立及有效成分含量测定[J].河南师范大学学报(自然科学版),2018,46(4):60
XU WQ, WEI XT, MA QQ, et al. HPLC-PAD fingerprint of Xiao’er Chiqiao Qingre granules and determination of functional components[J].J Henan Norm Univ(Nat Sci Ed), 2018,46(4):60
[12] 李超, 田刚, 吴菲,等. GC法同时测定小儿豉翘清热颗粒中9种挥发性成分[J].中成药, 2019, 41(4):739
LI C,TIAN G,WU F, et al. Simultaneous determination of nine volatile constituents in Xiao’er Chiqiao Qingre granules by GC[J].Chin Tradit Pat Med,2019, 41(4):739
[13] 周雯婷, 任美婷, 乐健, 等. LC-MS/MS法同时测定知母提取物中7种成分的含量[J].中国医药工业杂志, 2020,51(8):1036
ZHOU WT, REN MT, LE J, et al. Simultaneous determination of seven components in Anemarrhena asphodeloides extract by liquid chromatography-tandemtography-tandem[J].Chin J Pharm, 2020, 51(8):1036
[14] 孙大赢, 赵文法, 李广华, 等. LC-MS/MS法同时测定参芍胶囊中人参皂苷和芍药苷的含量[J].药物分析杂志, 2018, 38(1):186
SUN DY, ZHAO WF, LI GH, et al. Simultaneous determination of ginsenosides and paeoniflorin in Shenshao capsules by LC-MS/MS[J].Chin J Pharm Anal, 2018, 38(1):186
[15] 王献瑞, 赵西子, 王晓明, 等. 固相萃取LC-MS/MS法测定疏血通注射液中次黄嘌呤浓度[J].天津中医药大学学报, 2019,38(5):478
WANG XR, ZHAO XZ, WANG XM, et al. SPE-LC-MS/MS method for determination of hypoxanthine concentration in Shuxuetong injection[J].J Tianjin Univ Tradit Chin Med, 2019,38(5):478
[16] 徐绍娣, 崔宝国, 赵桂香, 等. LC-MS/MS同时测定刺五加中刺五加苷E、异嗪皮啶、绿原酸、原儿茶酸和齐墩果酸的含量[J].植物学研究, 2017, 6(4): 201
XU SD, CUI BG, ZHAO GX, et al. Simultaneous determination of eleutheroside E, isothiazine, chlorogenic acid, protocatechuic acid and oleanolic acid in Acanthopanax by LC-MS/MS[J].Bot Res, 2017, 6(4): 201
[17] 谢艳香, 姜二岗, 戴天明,等. LC-MS/MS同时测定鸡矢藤提取物中4个主要有效成分的含量[J].中国实验方剂学杂志, 2018,24(18): 57
XIE YX, JIANG EG, DAI TM, et al. Simultaneous determination of four main effective components in Paederia scandens extracts by LC-MS/MS[J].Chin J Exp Tradit Med Form, 2018,24(18):57
[18] 黄明萍, 谢水林, 戴仁科. LC-MS/MS同时测定复方救必应胶囊中3种同分异构体的含量[J].广东药科大学学报, 2018, 34(6):695
HUANG MP, XIE SL, DAI RK. Simultaneous determination of three isomers in compound Jiubiying capsules by LC-MS/MS[J].J Guangdong Pharm Univ, 2018, 34(6):695
[19] 白玮, 孙晓, 许苗苗, 等. LC-MS/MS同时测定窝儿七中10种成分的含量[J].中国实验方剂学杂志, 2018,24(18):63
BAI W, SUN X, XU MM, et al. Simultaneous determination of ten components in Diphylleia sinensis by LC-MS/MS[J].Chin J Exp Tradit Med Form, 2018,24(18): 63
[20] 吴文杰,刘良红,黄莺.LC-MS/MS法同时测定葛根药材中14种异黄酮类成分的含量[J].中国药房,2018,29(10):1320
WU WJ, LIU LH, HUANG Y. Simultaneous determination of 14 kinds of isoflavones in Pueraria radix by LC-MS/MS[J].China Pharm, 2018, 29(10):1320
