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UPLC-MS/QAMS测定小鼠血浆中石斛碱及其代谢产物M-250、M-280的浓度
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| 篇名： | UPLC-MS/QAMS测定小鼠血浆中石斛碱及其代谢产物M-250、M-280的浓度 |
| TITLE： | |
| 摘要： | 目的：首次建立测定小鼠血浆中石斛碱及其代谢产物M-250、M-280浓度的方法。方法：小鼠灌胃石斛碱60 mg/kg，1 h后收集血浆处理后，以盐酸伪麻黄碱为内标，以石斛碱对照品为对照，采用超高效液相色谱-质谱/一测多评法测定石斛碱及其代谢产物M-250、M-280的血药浓度。色谱柱为Hypersil Gold C18，流动相为0.1％甲酸水溶液-乙腈（梯度洗脱），流速为0.3 mL/min，柱温为40 ℃，进样量为5 μL；采用可加热电喷雾离子源，全扫描/正离子模式，雾化温度为300 ℃，离子传输管温度为350 ℃，鞘气流速为35 arb，辅助气流速为15 arb，喷雾电压为3.5 kV，碰撞电压为30、40、50 eV，质荷比检测范围为100～1 500。结果：小鼠血浆中内源性物质对石斛碱及其代谢产物M-250、M-280浓度测定无干扰；石斛碱检测质量浓度线性范围为9.13～912.94 ng/mL（r＝0.999 6）；定量下限为3.04 ng/mL，日内、日间精密度的RSD≤7.5％（n＝5或n＝3）；准确度为96.8％～107.5％（n＝5）；基质效应为97.1％～106.0％（RSD＝1.8％～4.7％，n＝5）；质控血浆样品溶液15 ℃保存24 h、－70 ℃保存并反复冻融3次以及－70 ℃保存15 d后浓度的RSD≤12.8％（n＝3）。小鼠血浆样品中石斛碱质量浓度为（41.3±5.7） ng/mL（n＝12），以相对校正因子（RCF）按1.0计，代谢产物M-250、M-280的质量浓度分别为（493.0±73.1）、（41.4±3.0） ng/mL（n＝12）。结论：该方法灵敏、准确，可用于小鼠血浆中石斛碱及其代谢产物M-250、M-280的浓度测定。 |
| ABSTRACT： | OBJECTIVE： To establish a method for the determination of dendrobine and its metabolites M-250 and M-280 in mice plasma for the first time. METHODS： Mice were given dendrobine 60 mg/kg by intragastric administration， 1 h later plasma were collected and treated. Using pseudoephedrine hydrochloride as internal standard and dendrobine reference substance as control， the plasma concentrations of dendrobine and its metabolites M-250 and M-280 were determined by UPLC-MS combined with quantitative analysis of multi-components by single marker. The separation was performed on Hypersil Gold C18 column with 0.1％ formic acid-acetonitrile （gradient elution） at the flow rate of 0.3 mL/min. The column temperature was set at 40℃， and sample size was 5 μL. Heatable electrospray ionization （HESI） source， scan/ESI+ were applied and operated in positive ion mode with atomization temperature of 300 ℃， ion transmission tube temperature of 350 ℃， the sheath gas velocity of 35 arb， the auxiliary air velocity of 15 arb， the spray voltage of 3.5 kV， the collision voltage of 30， 40， 50 eV. The mass-to-charge ratio of detection range were 100-1 500. RESULTS： The endogenous substances of mice plasma had no interference with the content determination of dendrobine and its metabolites M-250 and M-280. The linear range of dendrobine were 9.13-912.94 ng/mL （r＝0.999 6）. The limit of quantitation was 3.04 ng/mL. RSDs of intra-day and inter-day were all less than 7.5％ （n＝5 or n＝3）. The accuracy were 96.8％-107.5％ （n＝5）. Matrix effects were 97.1％-106.0％（RSD＝1.8％-4.7％，n＝5）. RSDs of the content of sample at 15℃ for 24 h， at －70 ℃ after three times freeze-thaw， at －70 ℃ for 15 d were lower than 12.8％ （n＝3）. The content of dendrobine in plasma sample of mice was （41.3±5.7） ng/mL（n＝12）. The contents of its metabolites M-250 and M-280 were （493.0±73.1） and （41.4±3.0） ng/mL （n＝12） with Relative correction factor of 1.0. CONCLUSIONS： The method is sensitive and accurate， and can be used for content determination of dendrobine and its metabolites M-250 and M-280 in mice plasma. |
| 期刊： | 2018年第29卷第11期 |
| 作者： | 鲁艳柳，黄思，刘浩，曾瑶，王建秋，徐亚沙，陆远富，何芋岐 |
| AUTHORS： | LU Yanliu，HUANG Si，LIU Hao，ZENG Yao，WANG Jianqiu，XU Yasha，LU Yuanfu，HE Yuqi |
| 关键字： | 石斛碱；代谢产物；M-250；M-280；小鼠；超高效液相色谱-质谱法；一测多评法 |
| KEYWORDS： | Dendrobine； Metabolites； M-250；M-280； Mice； UPLC-MS； Quantitative analysis of multi-components with single marker |
| 阅读数： | 306 次 |
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