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不同厂家八宝惊风散中人工牛黄胆汁酸类活性成分的含量测定及差异分析
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| 篇名： | 不同厂家八宝惊风散中人工牛黄胆汁酸类活性成分的含量测定及差异分析 |
| TITLE： | Determination and difference analysis of bile acid active constituents of artificial bezoar in Babao jingfeng powder from different manufacturers |
| 摘要： | 目的 建立同时测定八宝惊风散中人工牛黄有效成分（胆酸、猪去氧胆酸和牛磺胆酸钠）含量的方法，比较不同厂家样品中3个成分的含量差异。方法采用超高效液相串联质谱法测定3个厂家9批八宝惊风散中胆酸、猪去氧胆酸和牛磺胆酸钠的含量，色谱柱为PhenomenexLuna®C18，流动相为乙腈-水（梯度洗脱），流速为0.5mL/min，柱温为40℃，进样量为2μL。质谱采用负离子单四极杆模式，胆酸、猪去氧胆酸和牛磺胆酸钠的m/z分别为407.2、392.2、514.2。以3个成分的含量为指标，对9批样品进行聚类分析和主成分分析。结果胆酸、猪去氧胆酸和牛磺胆酸钠的线性范围分别为5.48～548.40、5.38～538.40、4.74～474.05ng/mL（r≥0.9993）；精密度、重复性、稳定性（24h）的RSD均不高于3.7%（n＝6），平均回收率分别为103.3%、103.3%、101.6%，RSD分别为3.3%、3.4%、4.2%（n＝6）。9批样品中胆酸、猪去氧胆酸、牛磺胆酸钠的含量分别为0.702～1.711、0.599～2.049、0.664～1.752mg/g。A厂家样品中3个成分的平均含量较高，批间差异最小；C厂家样品中3个成分的平均含量最低，批间差异较大。聚类分析基本可以区分不同厂家的样品；以主成分综合得分为指标进行聚类分析，结果与含量聚类分析结果基本一致。结论成功建立了同时测定八宝惊风散中人工牛黄3个胆汁酸类有效成分含量的方法。各厂家样品中3个成分的含量存在较大差异。 |
| ABSTRACT： | OBJECTIVE To establish the method for determination of bile acid active constituents （cholic acid， hyodeoxycholic acid and sodium taurocholate） in Babao jingfeng powder， and to compare the differences of 3 constituents in Babao jingfeng powder from different manufacturers. METHODS UPLC-MS method was adopted to determine the contents of cholic acid， hyodeoxycholic acid and sodium taurocholate in 9 batches of Babao jingfeng powder from 3 manufacturers. The separation was performed on a Phenomenex Luna® C18 column with mobile phase consisted of acetonitrile-water （gradient elution） at a flow rate of 0.5 mL/min. The column temperature was 40 ℃ and the sample size was 2 μL. MS system was operated in a negative ion single quadrupole mode， and the m/z of cholic acid， hyodeoxycholic acid and sodium taurocholate were 407.2， 392.2 and 514.2， respectively. With the contents of three components as the index， cluster analysis and principle component analysis were performed on 9 batches of samples. RESULTS The linear ranges of cholic acid， hyodeoxycholic acid and sodium taurocholate were 5.48- 548.40， 5.38-538.40， 4.74-474.05 ng/mL， respectively （r≥ 0.999 3）. RSDs of precision， repeatability and stability tests（24 h） were all lower than or equal to 3.7% （n＝6）， and the average recoveries were 103.3%， 103.3% and 101.6% with RSDs of 3.3%， 3.4%， 4.2% （n＝6）， respectively. The contentsof cholic acid ranged 0.702-1.711 mg/g， those of deoxycholic acid ranged 0.599-2.049 mg/g， and those of sodium taurocholate ranged 0.664-1.752 mg/g in 9 batches of samples. The average content of 3 components in samples from manufacturer A was high， and the difference between batches was the smallest； the average content of 3 components from manufacturer C was the lowest， and the difference between batches was large. Cluster analysis could basically distinguish samples from different manufacturers； cluster analysis was conducted by using the comprehensive score of principal components as an indicator， the results of which were basically consistent with those of cluster analysis for content. CONCLUSIONS The method is established successfully for the content determination of the 3 bile acid active constituents of artificial bezoar in Babao jingfeng powder. The contents of 3 components in Babao jingfeng powder from 3 manufacturers are significantly different. |
| 期刊： | 2023年第34卷第20期 |
| 作者： | 钟琪；陈伟康；周国平；刘艳梅；刘德鸿；李晶 |
| AUTHORS： | ZHONG Qi，CHEN Weikang，ZHOU Guoping，LIU Yanmei，LIU Dehong，LI Jing |
| 关键字： | 八宝惊风散；胆酸；猪去氧胆酸；牛磺胆酸钠；人工牛黄；含量测定 |
| KEYWORDS： | Babao jingfeng powder； cholic acid； hyodeoxycholic acid； sodium taurocholate； artificial bezoar； content |
| 阅读数： | 36 次 |
| 本月下载数： | 4 次 |
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