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银黄吸入溶液的指纹图谱建立及酚酸类成分的含量测定
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| 篇名： | 银黄吸入溶液的指纹图谱建立及酚酸类成分的含量测定 |
| TITLE： | Establishment of the fingerprints of Yinhuang solution for inhalation and content determination of phenolic acids |
| 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0.0250～1.2474μg（r＝0.9997）、0.0393～1.1787μg（r＝0.9999）、0.0316～1.1841μg（r＝0.9999）；精密度、重复性、稳定性（48h）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0.3018～0.3863、0.2625～0.3625mg/mL，外标法测得新绿原酸、绿原酸、隐绿原酸含量分别为0.3026～0.3872、0.2310～0.3340、0.2616～0.3613mg/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。 |
| ABSTRACT： | OBJE CTIVE To establish the finger prints 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 acid and cryptochlorogenic acid by ESM were 0.302 6-0.387 2， 0.231 0- 0.334 0，0.261 6-0.361 3 mg/mL，respectively. The deviations of the content determination results of the two methods（except for chlorogenic acid ）were both not higher than 0.20％. CONCLUSIONS Established HPLC fingerprints are stable and feasible. Established QAMS method is accurate and rapid. HPLC fingerprint combined with QAMS can be used for the quality control for Yinhuang solution for inhalation ． |
| 期刊： | 2022年第33卷第02期 |
| 作者： | 高进，李翠，尹睿卓，马新称，王慧阳，龚春晖，陈承瑜，曹晖 |
| AUTHORS： | GAO Jin，LI Cui，YIN Ruizhuo ，MA Xincheng ，WANG Huiyang ，GONG Chunhui ，CHEN Chengyu ，CAO Hui |
| 关键字： | 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 |
| KEYWORDS： | Yinhuang solution for inhalation ； high performance liquid chromatography ； fingerprint； phenolic acids ； |
| 阅读数： | 175 次 |
| 本月下载数： | 7 次 |
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