芪芎左归颗粒中龟甲胶、鹿角胶的鉴别及12种化学成分的含量测定  

Identification of tortoiseshell glue and antler glue in Qixiong zuogui granules and content determination of 12 chemical components

作　　者：贾孟晓 常春辉 刘洋[1] 王雅倩 张运克 贾永艳[1,3] JIA Mengxiao;CHANG Chunhui;LIU Yang;WANG Yaqian;ZHANG Yunke;JIA Yongyan(College of Pharmacy,Henan University of Chinese Medicine,Zhengzhou 450046,China;School of Rehabilitation Medicine,Henan University of Chinese Medicine,Zhengzhou 450046,China;Henan Engineering Research Center of Traditional Chinese Medicine Processing Technology,Zhengzhou 450046,China)

机构地区：[1]河南中医药大学药学院,郑州450046 [2]河南中医药大学康复医学院,郑州450046 [3]河南省中药特色炮制技术工程研究中心,郑州450046

出　　处：《中国药房》2025年第5期540-545,共6页China Pharmacy

基　　金：国家自然科学基金项目(No.81974564);河南省高等学校重点科研项目(No.20B360003);河南省“双一流”创建学科中医学科学研究专项(No.HSRP-DFCTCM-2023-1-04)。

摘　　要：目的鉴别芪芎左归颗粒中的龟甲胶、鹿角胶,并对该制剂中12种化学成分进行含量测定。方法采用液相色谱串联质谱法进行鉴别和含量测定。鉴别过程所用色谱柱为Hypersil GOLD,流动相为乙腈-0.1%甲酸溶液(梯度洗脱),采用电喷雾离子源,以正离子多反应检测模式扫描,质荷比(m/z)631.3→546.4、631.3→921.4为龟甲胶的检测离子对,m/z 765.4→554.0、765.4→733.0为鹿角胶的检测离子对。含量测定过程所用色谱柱为Accucore C_(18),流动相为甲醇-0.1%甲酸溶液(梯度洗脱),采用电喷雾离子源,以单离子检测模式扫描,正、负离子扫描范围均为m/z 100→1000。结果龟甲胶、鹿角胶特征肽段分子离子峰的平均保留时间分别为6.28、6.77 min。黄芪甲苷、毛蕊异黄酮苷、毛蕊异黄酮、绿原酸、阿魏酸、甜菜碱、苦杏仁苷、芦丁、羟基红花黄色素A、金丝桃苷、马钱苷、杯苋甾酮这12种化学成分在各自质量浓度范围内线性关系良好(r>0.999),精密度、稳定性(24 h)和重复性的RSD均小于5%,平均加样回收率为98.04%~101.08%,平均含量分别为1.83、25.73、13.76、56.71、23.80、49.82、807.49、15.01、317.02、60.21、202.71、17.70μg/g。结论本研究鉴别了芪芎左归颗粒中的龟甲胶和鹿角胶,并对制剂中12种化学成分进行了含量测定,可为该制剂的质量控制提供参考。OBJECTIVE To identify tortoiseshell glue and antler glue in Qichong zuogui granules,and determine the contents of 12 chemical components.METHODS Identification and content determination were performed by using liquid chromatographytandem mass spectrometry(LC-MS/MS)method.The identification was performed on Hypersil GOLD column with a mobile phase consisted of acetonitrile-0.1%formic acid solution(gradient elution);the electrospray ion source was used to scan in the positive ion multi-reaction detection mode.The mass charge ratio(m/z)631.3→546.4,631.3→921.4 was the detection ion pair for tortoiseshell glue,and the m/z 765.4→554.0,765.4→733.0 was the detection ion pair for antler glue.The determination method for 12 chemical components was as follows:Accucore C_(18) column,methanol-0.1%formic acid as mobile phase(gradient elution);scanning range of positive and negative ions was m/z 100→1000 with the electric spray ion source and single ion detection scanning mode.RESULTS Average retention times of the molecular ion peaks for characteristic peptide segments of tortoiseshell glue and antler glue were 6.28 and 6.77 min,respectively;the linear relationship of 12 chemical components was good within their respective concentration ranges,such as astragalosideⅣ,calycosin-7-O-β-D-glucoside,calycosin,chlorogenic acid,ferulic acid,betaine,amygdalin,rutin,hydroxysafflor yellow A,hyperoside,loganin,cyasterone(r>0.999);RSDs for precision,stability(24 h)and reproducibility tests were all less than 5%.The average sample recovery rates ranged from 98.04%to 101.08%.The average contents of 12 components were 1.83,25.73,13.76,56.71,23.80,49.82,807.49,15.01,317.02,60.21,202.71 and 17.70μg/g,respectively.CONCLUSIONS In this study,tortoiseshell glue and antler glue in Qixiong zuogui granules are identified,and the contents of 12 chemical components therein are determined.This provides a reference for the quality control of this granule.

关 键 词：芪芎左归颗粒 龟甲胶 鹿角胶 鉴别 含量测定 液相色谱串联质谱 

分 类 号：R917[医药卫生—药物分析学] R284.1[医药卫生—药学]