Page 38 - 《中国药房》2022年2期

银黄吸入溶液的指纹图谱建立及酚酸类成分的含量测定 Δ

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高 进 1，2＊ ，李 翠 ，尹睿卓 ，马新称 ，王慧阳 ，龚春晖 ，陈承瑜 ，曹 晖 [1.暨南大学药学院，广州
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510632；2.盈科瑞（横琴）药物研究院有限公司/国家中药现代化工程技术研究中心新型递药系统分中心/广东省
雾化吸入制剂工程技术研究中心，广东 珠海 519000]
中图分类号 R284.1 文献标志码 A 文章编号 1001-0408（2022）02-0160-05
DOI 10.6039/j.issn.1001-0408.2022.02.06
摘 要 目的 建立银黄吸入溶液的指纹图谱，并同时测定新绿原酸、绿原酸、隐绿原酸的含量。方法 以黄芩苷为参照峰，采用高
效液相色谱（HPLC）法建立银黄吸入溶液的指纹图谱；以绿原酸为参照物，采用斜率校正法计算新绿原酸、隐绿原酸的相对校正因
子，再根据相对校正因子计算两者的含量，并将上述一测多评（QAMS）法的检测结果与外标法进行比较。结果 10批银黄吸入溶
液共有18个共有峰，与对照指纹图谱的相似度均大于0.90；共指认了7个共有峰，分别为黄芩苷、新绿原酸、绿原酸、隐绿原酸、异
绿原酸B、3，5-二-O-咖啡酰奎宁酸和4，5-二-O-咖啡酰奎宁酸。新绿原酸、绿原酸、隐绿原酸检测进样量的线性范围分别为0.025 0～
1.247 4 μg（r＝0.999 7）、0.039 3～1.178 7 μg（r＝0.999 9）、0.031 6～1.184 1 μg（r＝0.999 9）；精密度、重复性、稳定性（48 h）试验的
RSD 均小于 1.0％；平均加样回收率分别为 93.92％（RSD＝1.32％，n＝6）、94.46％（RSD＝1.45％，n＝6）、93.93％（RSD＝1.57％，
n＝6）。新绿原酸、隐绿原酸相对于绿原酸的相对校正因子分别为 1.068、1.233。QAMS 法测得新绿原酸、隐绿原酸含量分别为
0.301 8～0.386 3、0.262 5～0.362 5 mg/mL，外标法测得新绿原酸、绿原酸、隐绿原酸含量分别为0.302 6～0.387 2、0.231 0～0.334 0、
0.261 6～0.361 3 mg/mL；两种方法含量测定结果（绿原酸除外）的偏差均不高于0.20％。结论 所建HPLC指纹图谱稳定、可行，所
建QAMS法准确、重复性好；HPLC指纹图谱结合QAMS法可用于银黄吸入溶液的质量控制。
关键词 银黄吸入溶液；高效液相色谱法；指纹图谱；酚酸类成分；一测多评法；含量测定

Establishment of the fingerprints of Yinhuang solution for inhalation and content determination of phenolic
acids
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GAO Jin ，LI Cui ，YIN Ruizhuo ，MA Xincheng ，WANG Huiyang ，GONG Chunhui ，CHEN Chengyu ，
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CAO Hui [1. College of Pharmacy，Jinan University，Guangzhou 510632，China；2. Increasepharm（Hengqin）
Institute Co.，Limited/National Engineering Research Center for Modernization of Traditional Chinese Medicine
New Drug Delivery System Branch/Guangdong Province Engineering Research Center for Aerosol Inhalation
Preparation，Guangdong Zhuhai 519000，China]
ABSTRACT OBJECTIVE To establish the fingerprints for Yinhuang solution for inhalation and determine the contents of
neochlorogenic acid，chlorogenic acid and cryptochlorogenic acid simultaneously. METHODS Using baicalin as reference，the
fingerprints of Yinhuang solution for inhalation were established by high performance liquid chromatography （HPLC）. Relative
correction factors of neochlorogenic acid and cryptochlorogenic acid were calculated by slope correction method，using chlorogenic
acid as reference；the contents of them were calculated according to relative correction factor. The results of quantitative analysis of
multi-components by single marker（QAMS）were compared with those of external standard method（ESM）. RESULTS There
were 18 common peaks in the fingerprints of 10 batches of Yinhuang solution for inhalation，and their similarities with reference
fingerprint were higher than 0.90. A total of 7 common peaks were identified as baicalin，neochlorogenic acid，chlorogenic acid，
cryptochlorogenic acid，isochlorogenic acid B，3，5-di-O-caffeoylquinic acid and 4，5-di-O-caffeoylquinic acid. The linear range of
neochlorogenic acid，chlorogenic acid and cryptochlorogenic acid were 0.025 0-1.247 4 μg（r＝0.999 7），0.039 3-1.178 7 μg（r＝
0.999 9），0.031 6-1.184 1 μg（r＝0.999 9），respectively. RSDs of precision，reproducibility and stability tests（48 h）were all
lower than 1.0％. The average recoveries were 93.92％（RSD＝1.32％ ，n＝6），94.46％（RSD＝1.45％，n＝6），93.93％（RSD＝
1.57％，n＝6）. Relative correction factors of neochlorogenic acid and cryptochlorogenic acid were 1.068 and 1.233. The contents of
neochlorogenic acid and cryptochlorogenic acid determined by QAMS method were 0.301 8-0.386 3 and 0.262 5-0.362 5 mg/mL，
respectively. The contents of neochlorogenic acid，chlorogenic
Δ 基金项目：“重大新药创制”科技重大专项（No.2017ZX09201002）；
acid and cryptochlorogenic acid by ESM were 0.302 6-0.387 2，
广东省省级科技计划项目（No.2020A050515006）
0.231 0- 0.334 0，0.261 6-0.361 3 mg/mL，respectively. The
＊副主任中药师，博士。研究方向：药物制剂与中药新药研发。
电话：0756-6969103。E-mail：172078415@qq.com deviations of the content determination results of the two
# 通信作者：教授，博士。研究方向：岭南中药资源的品质评价与 methods （except for chlorogenic acid） were both not higher
药材标准。电话：0756-8135676。E-mail：kovhuicao@aliyun.com than 0.20％. CONCLUSIONS Established HPLC fingerprints

·160 · China Pharmacy 2022 Vol. 33 No. 2 中国药房 2022年第33卷第2期