小儿健脾颗粒质量标准建立研究  

Establishment of quality standard of Xiao’er Jianpi Granules

作　　者：王鼎 王佳 胡军华[2,3] 章晨峰 王振中[1,2,3] 林夏 肖伟[1,2,3] WANG Ding;WANG Jia;HU Jun-hua;ZHANG Chen-feng;WANG Zhen-zhong;LIN Xia;XIAO Wei(Nanjing University of Chinese Medicine,Nanjing 210000,China;Jangsu Kanion Pharmaceutical Co.,Ltd.,Lianyungang 222001,China;National Key Laboratory on Technologies for Chinese Medicine Pharmaceutical Process Control and Intelligent Manufacture,Lianyungang 222001,China)

机构地区：[1]南京中医药大学,江苏南京210000 [2]江苏康缘药业股份有限公司,江苏连云港222001 [3]中药制药过程控制与智能制造技术全国重点实验室,江苏连云港222001

出　　处：《中草药》2023年第18期5933-5940,共8页Chinese Traditional and Herbal Drugs

基　　金：国家中医药管理局—基于重点研究室研究领域的中医药多学科研究能力提升项目:中药提取精制新技术。

摘　　要：目的建立小儿健脾颗粒(Xiao’er Jianpi Granules,XJG)的定性、定量分析方法。方法采用TLC法,以“整体鉴别”新模式为基础,建立了一样多测(炒莱菔子、甘草及陈皮)及一板多鉴(炒莱菔子、甘草)的鉴别方法。采用HPLC法,采用Kromasil C18色谱柱(150 mm×4.6 mm,3.5μm),以0.1%三氟乙酸-乙腈为流动相进行梯度洗脱,进样量5μL,柱温30℃,体积流量1 mL/min,检测波长252 nm(甘草酸)、275 nm(甘草苷)、283 nm(芸香柚皮苷、橙皮苷)、326 nm(3,6′-二芥子酰基蔗糖、芥子碱硫氰酸盐)。结果建立的TLC鉴别方法,斑点清晰,能专属的鉴别处方中白术、陈皮、山药、炒莱菔子、焦山楂、甘草;建立了芥子碱硫氰酸盐、3,6′-二芥子酰基蔗糖、橙皮苷、芸香柚皮苷、甘草苷、甘草酸含量测定方法,6个成分在各自质量浓度范围内线性关系良好(r≥0.9999),精密度、稳定性及重复性良好,加样回收率为97.8%~101.6%;4批样品中芥子碱硫氰酸盐、3,6′-二芥子酰基蔗糖、橙皮苷、芸香柚皮苷、甘草苷、甘草酸的质量浓度分别为0.57~0.80、0.44~0.64、3.81~4.93、1.45~2.72、0.56~1.14、1.20~1.58 mg/mL。结论建立了6个药味的TLC鉴别方法,斑点清晰且专属性强。建立了HPLC同时测定的6个成分含量测定方法,建立的方法快速、准确、专属性强,为其质量标准建立提供参考依据。Objective To establish a qualitative and quantitative analysis method for Xiao’er Jianpi Granules(小儿健脾颗粒,XJG).Methods Based on the new pattern of“holistic identification”,TLC was used to establish the identification methods of one-sample multi-detection[stir-fried Laifuzi(Raphani Semen,sRS),Gancao(Glycyrrhizae Radix et Rhizoma,GRR)and Chenpi(Citri Reticulatae Pericarpium,CRP)]and one-plate multi-detection(sRS,GRR).HPLC was performed on a Kromasil C18 column(150 mm×4.6 mm,3.5μm)with a gradient elution using 0.1%trifluoroacetic acid-acetonitrile as the mobile phase,the injection volume was 5μL,the column temperature was 30℃,the flow rate was 1 mL/min,and the detection wavelengths were 252 nm(glycyrrhizic acid),275 nm(liquiritin),283 nm(narirutin,hesperidin),326 nm(3,6′-disinapoyl sucrose,sinapine thiocyanate).Results The established TLC identification methods with clear spots,could exclusively identify Baizhu(Atractylodis Macrocephalae Rhizoma,AMR),CRP,Shanyao(Dioscoreae Rhizoma,DR),sRS,Shanzha(Crataegi Fructus,CF)and GRR in the prescription.A method was established for the determination of sinapine thiocyanate,3,6′-dierosyl sucrose,hesperidin,narirutin,liquiritin and glycyrrhizic acid,the linear relationship of the six main components in their respective concentration ranges was good(r≥0.9999)and the precision,stability and repeatability were good.The recoveries were 97.8%-101.6%.The mass concentrations of sinapine thiocyanate,3,6′-dierosyl sucrose,hesperidin,narirutin,liquiritin and glycyrrhizic acid in four batches of sample were 0.57-0.80,0.44-0.64,3.81-4.93,1.45-2.72,0.56-1.14,1.20-1.58 mg/mL,respectively.Conclusion The TLC method for the identification of six medicinal flavors was established,and the identification was clear and exclusive.The HPLC method for the simultaneous determination of six components was established.The established method is rapid,accurate and specific,which provides a reference basis for the establishment of quality standards.

关 键 词：小儿健脾颗粒 HPLC TLC 一板多鉴法 质量控制 整体鉴别 一样多测 甘草酸 甘草苷 芸香柚皮苷 橙皮苷 3 6′-二芥子酰基蔗糖 芥子碱硫氰酸盐 白术 陈皮 山药 炒莱菔子 山楂 甘草 

分 类 号：R283.6[医药卫生—中药学]