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复方硫酸软骨素片中6种乌头碱类成分的含量测定及质量评价
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| 篇名： | 复方硫酸软骨素片中6种乌头碱类成分的含量测定及质量评价 |
| TITLE： | Content determination of six Aconitum alkaloids and quality evaluation in Compound chondroitin sulfate tablets |
| 摘要： | 目的 建立同时测定复方硫酸软骨素片中6种乌头碱类成分含量的超高效液相色谱-串联质谱（UPLC-MS/MS）法，并对不同批次样品进行质量评价，为该制剂的质量控制提供参考。方法采用AgilentSB-C18色谱柱分离，以0.2%甲酸（氨水调pH至7.5）-乙腈为流动相进行梯度洗脱，流速为0.3mL/min，柱温为35℃，进样量为1μL；质谱采用AJSESI+离子源、多反应监测模式，以外标法定量；并进行方法学考察。应用所建UPLC-MS/MS法对来自3家生产企业的64批样品中6种乌头碱类成分（包括乌头碱、次乌头碱、新乌头碱3种双酯型生物碱和苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱3种单酯型生物碱）的含量进行测定；采用描述性统计分析、Kruskal-WallisH检验、主成分分析（PCA）和Spearman秩相关分析分别评价乌头碱类成分的含量分布、不同生产企业间样品差异及成分之间的相关性。结果6种乌头碱类成分在各自质量浓度范围内线性关系良好（r均大于0.99）；精密度、重复性、稳定性考察的RSD均小于5%，方法的检测限和定量限分别不高于0.003ng/mL和0.01ng/mL；平均加样回收率为96.43%～102.30%，RSD为0.35%～4.92%。64批样品中单酯型生物碱类成分的总量（均值为0.0349mg/片）明显高于双酯型生物碱类成分总量（均值为0.0022mg/片），其中苯甲酰新乌头原碱含量最高（均值为0.0310mg/片），其余5种成分含量均较低，且批间变异较大；不同生产企业样品间各成分含量差异无统计学意义（P＞0.05），PCA未显示明显聚类趋势，部分成分之间存在显著相关性（P＜0.05）。结论所建UPLC-MS/MS方法可同时快速、准确地测定复方硫酸软骨素片中上述6种乌头碱类成分的含量；多批次样品质量评价可为该制剂的质量控制提供参考。 |
| ABSTRACT： | OBJECTIVE To establish an ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for the simultaneous determination of the contents of six Aconitum alkaloids in Compound chondroitin sulfate tablets， and to perform quality evaluation of samples from different batches， thereby providing a reference for the quality control of this preparation.METHODS Chromatographic separation was performed on an Agilent SB-C 18 column using gradient elution with 0.2% formic acid （adjusted to pH 7.5 with ammonia） and acetonitrile as the mobile phases. The flow rate was 0.3 mL/min， the column temperature was 35 ℃， and the injection volume was 1 μL. Mass spectrometric analysis was performed using an AJS ESI + ion source in multiple reaction monitoring mode， with quantification by the external standard method. Method validation was performed. The established UPLC-MS/MS method was applied to determine the contents of the six Aconitum alkaloids in 64 batches of samples from three manufacturers， including three diester-type alkaloids （aconitine， hypaconitine， and mesaconitine） and three monoester-type alkaloids （benzoylaconine， benzoylhypaconine， and benzoylmesaconine）. Descriptive statistics， the Kruskal-Wallis H test， principal component analysis （PCA）， and Spearman’s rank correlation analysis were used to evaluate the content distribution of Aconitum alkaloids， differences among samples from different manufacturers， and correlations among the components.RESULTS Good linearity was observed for the six Aconitum alkaloids over their respective concentration ranges， with correlation coefficients （all r ＞0.99）. The relative standard deviations （RSDs） for precision， repeatability， and stability were all less than 5%. The limits of detection and quantification were no higher than 0.003 ng/mL and 0.01 ng/mL， respectively. The mean recoveries ranged from 96.43% to 102.30%， with RSDs ranging from 0.35% to 4.92%. Among the 64 batches of samples， the total content of monoester-type alkaloids （mean value of 0.034 9 mg/tablet） was markedly higher than that of diester-type alkaloids （mean value of 0.002 2 mg/tablet）. Benzoylmesaconine showed the highest content， with a mean value of 0.031 0 mg/tablet， whereas the other five components were present at relatively low levels and showed considerable inter-batch variation. No statistically significant differences were observed in the contents of the six components among samples from different manufacturers （ P ＞0.05）. PCA showed no obvious clustering trend， and significant correlations were observed among some components （ P ＜0.05）.CONCLUSIONS The established UPLC-MS/MS method enables the rapid and accurate simultaneous determination of the above-mentioned six Aconitum alkaloids in Compound chondroitin sulfate tablets. The quality evaluation of multiple batches of samples provides a reference for the quality control of this preparation. |
| 期刊： | 2026年第37卷第19期 |
| 作者： | 章璐璐；叶佳；朱雪梅；杨恩慈 |
| AUTHORS： | ZHANG Lulu，YE Jia，ZHU Xuemei，YANG Enci |
| 关键字： | 复方硫酸软骨素片;乌头碱类成分;超高效液相色谱-串联质谱法;含量测定;附子;质量评价 |
| KEYWORDS： | Compound chondroitin sulfate tablets; Aconitum alkaloids;ultra-performance liquid chromatography-tandem mass spectrometry method;Content determination; Aconitum carmichaelii ;Quality evaluation |
| 阅读数： | 2 次 |
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