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UPLC-MS/MS法同时测定不同基原藏黄堇中3种生物碱的含量
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| 篇名： | UPLC-MS/MS法同时测定不同基原藏黄堇中3种生物碱的含量 |
| TITLE： | Content determination of 3 alkaloids in different origins of Tibetan Corydalis pallida by UPLC-MS/MS |
| 摘要： | 目的 建立并应用同时测定不同基原藏黄堇中荷包牡丹碱、原阿片碱、黄连碱含量的方法，为该类药材的基原确定和质量控制提供参考依据。方法采用超高效液相色谱-三重四极杆质谱联用（UPLC-MS/MS）法：色谱柱为AgilentEC-C18（100mm×2.1mm，2.7μm），以乙腈-0.1%甲酸水溶液为流动相梯度洗脱，流速为0.2mL/min，柱温为35℃。采用电喷雾离子源正离子模式检测，多反应监测扫描。结果荷包牡丹碱、原阿片碱、黄连碱的进样质量浓度分别在5.88～117.60、53.70～1074.00、4.85～97.00ng/mL之间与各自峰面积成良好的线性关系（r分别为0.9982、0.9919、0.9996）；定量限分别为2.35、1.07、1.46ng/mL，检测限分别为1.17、0.54、0.49ng/mL；精密度、稳定性（24h）、重复性试验的RSD均未超过2.0%；平均加样回收率分别为97.41%、98.89%、105.44%（RSD均小于5.0%，n＝6）。结论所建立的方法选择性好、准确度高，适用紫堇属植物中荷包牡丹碱、原阿片碱和黄连碱的快速分析。3种生物碱总量在不同基原药材中的含量从高到低依次为金球黄堇、尖突黄堇、矮黄堇、尼泊尔黄堇和斑花黄堇，其中金球黄堇和尖突黄堇中的生物碱含量比较接近，但斑花黄堇和尼泊尔黄堇中未检测到荷包牡丹碱。 |
| ABSTRACT： | OBJECTIVE To establish and apply a method for simultaneous determination of the contents of dicentrine， protopine and coptisine in Tibetan Corydalis pallida of different origins， and to provide reference for origin determination and quality control of the kind of medicinal materials. METHODS Ultra performance liquid chromatography-tandem quadrupole mass spectrometry method was used. The determination was performed on Agilent EC-C18 column （100 mm×2.1 mm， 2.7 μm） with mobile phase consisted of acetonitrile-0.1% formic acid by gradient elution. The flow rate was 0.2 mL/min， and the column temperature was set at 35 ℃ . MS detection was carried out by electrospray ionization in positive modes， multiple reaction monitoring mode was used for quantitative analysis. RESULTS The injection mass concentrations of dicentrine， protopine， coptisine ranged from 5.88 to 117.60， 53.70 to 1 074.00， and 4.85 to 97.00 ng/mL， respectively， showing a good linear relationship with their respective peak areas （r＝0.998 2， 0.991 9， and 0.999 6， respectively）. The limits of quantitation were 2.35， 1.07 and 1.46 ng/mL； the limits of detection were 1.17， 0.54， 0.49 ng/mL， respectively. RSDs of precision， stability （24 h） and repeatability tests were all lower than 2.0％. The average recovery rates were 97.41%， 98.89% and 105.44%（ all RSDs＜5.0％， n＝6）. CONCLUSIONS The established method has good selectivity and high accuracy， and is suitable for the rapid analysis of dicentrine， protopine and coptisine in Corydalis. The total contents of three alkaloids in different original medicinal materials are from high to low in order of C. chrysosphaera， C. mucronifera， C. pygmaea， C. hendersonii and C. conspersa. The alkaloid contents in C. chrysosphaera and C. mucronifera are relatively similar， but no dicentrine has been detected in C. conspersa and C. hendersonii. |
| 期刊： | 2023年第34卷第07期 |
| 作者： | 黄唤；易徐航；邱毅；熊永昌；王惠鹃；蔡志男；达娃卓玛；袁金斌 |
| AUTHORS： | HUANG Huan， YI Xuhang，QIU Yi，XIONG Yongchang，WANG Huijuan，CAI Zhinan，Dawa Zhuoma，YUAN Jinbin |
| 关键字： | 藏黄堇；超高效液相色谱-三重四极杆质谱联用法；荷包牡丹碱；原阿片碱；黄连碱；含量测定 |
| KEYWORDS： | Tibetan Corydalis pallida； ultra performance liquid chromatography-tandem quadrupole mass spectrometry method； |
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