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UPLC-MS/MS法同时测定同仁牛黄清心丸中15个胆汁酸的含量
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| 篇名： | UPLC-MS/MS法同时测定同仁牛黄清心丸中15个胆汁酸的含量 |
| TITLE： | Simultaneous determination of 15 bile acids in Tongren niuhuang qingxin pills by UPLC-MS/MS |
| 摘要： | 目的 建立同时测定同仁牛黄清心丸中15个胆汁酸成分含量的方法，并采用该法测定15批样品的含量。方法以脱氢胆酸为内标，采用超高效液相色谱-串联质谱（UPLC-MS/MS）技术进行测定。色谱柱为HypersilGOLDC18，以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱，流速为0.2mL/min，柱温为40℃，进样量为2µL；采用加热型电喷雾离子源，在负离子模式下进行平行反应监测模式扫描。采用SPSS24.0软件对含量测定结果进行化学模式识别分析。结果15个胆汁酸成分在各自检测质量浓度范围内与峰面积线性关系良好（R2均不小于0.9989），精密度、重复性、稳定性均良好（RSD均不大于5.49%），平均加样回收率为93.8%～105.7%（RSD为0.5%～5.8%）。牛磺胆酸、7-酮-3α，12α-羟基胆烷酸、12-脱氢胆酸、甘氨胆酸、3-oxo-7α，12α-hydroxy-5β-cholanoicacid、牛磺鹅脱氧胆酸、3α-羟基-7-氧代-5β-胆烷酸、猪胆酸、牛磺脱氧胆酸钠、猪脱氧胆酸、胆酸、甘氨鹅脱氧胆酸、甘氨脱氧胆酸、鹅脱氧胆酸、脱氧胆酸的平均含量分别为670.56、25.97、10.54、280.12、4.04、29.81、182.98、813.55、120.95、220.31、797.37、18.37、68.59、30.13、59.82μg/g。聚类分析和主成分分析均将15批同仁牛黄清心丸分为2类，其中S1～S12为一类，S13～S15为另一类。结论所建方法准确、灵敏度高、专属性强，且测定胆汁酸种类较多，能快速实现对同仁牛黄清心丸中15个胆汁酸成分的定量分析，适用于该药的质量控制。 |
| ABSTRACT： | OBJECTIVE To establish a method for simultaneous determination of 15 bile acids in Tongren niuhuang qingxin pills， and to determine the contents of 15 batches of samples. METHODS Using dehydrocholic acid as internal standard， the determination was performed by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method. The determination was performed on Hypersil GOLD C18 column with methanol-0.1% formic acid solution as the mobile phase by gradient elution at the flow rate of 0.2 mL/min. The column temperature was 40 ℃ ， and the sample size was 2 µL. Using heated electrospray ion source， parallel reaction monitoring mode scanning was performed in negative ion mode. SPSS 24.0 software was used for chemical pattern recognition analysis of content determination results. RESULTS The 15 bile acid components had a good linear relationship with peak area （all R2≥0.998 9）； their precision， repeatability and stability were all good （all RSD≤5.49%）； the average recoveries were 93.8%-105.7% （RSD was 0.5%-5.8%）. The average contents of taurocholic acid， 7-oxodeoxycholic acid， 12-dehydrocholic acid， glycocholic acid， 3-oxo-7α， 12α-hydroxy-5β-cholanoic acid， taurochenodeoxycholic acid， 3α-hydroxy- 7-oxo-5β -cholanic acid， hyocholic acid， taurodeoxycholic acid sodium salt hydrate， hyodeoxycholic acid， cholic acid， glycochenodeoxycholic acid， glycodeoxycholic acid， chenodeoxycholic acid and deoxycholic acid were 670.56， 25.97， 10.54， 280.12， 4.04， 29.81， 182.98， 813.55， 120.95， 220.31， 797.37， 18.37， 68.59， 30.13， 59.82 μg/g， respectively. Both cluster analysis and principal component analysis divided 15 batches of Tongren niuhuang qingxin pills into 2 categories， S1-S12 as one category and S13-S15 as the other category. CONCLUSIONS The established method is accurate， sensitive and specific， and can determine many types of bile acids. It also can quickly achieve the quantitative analysis of 15 bile acids in Tongren niuhuang qingxin pills， which is suitable for the quality control of this drug. |
| 期刊： | 2023年第34卷第17期 |
| 作者： | 陈雪婷；林诗铃；陈涛；林逸凡；黄鸣清；郑燕芳 |
| AUTHORS： | CHEN Xueting，LIN Shiling，CHEN Tao，LIN Yifan，HUANG Mingqing，ZHENG Yanfang |
| 关键字： | 同仁牛黄清心丸；超高效液相色谱-串联质谱法；胆汁酸；含量测定；化学模式识别分析 |
| KEYWORDS： | Tongren niuhuang qingxin pills； ultra-high performance liquid chromatography-tandem mass spectrometry； bile |
| 阅读数： | 43 次 |
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