液相色谱-串联质谱法分析贝母中异甾体生物碱成分
发布时间：2018-11-26 21:01
【摘要】：川贝母具有止咳化痰之功效,是经济价值较高的药品,因此市场上偶有将低价格贝母掺入其中的行为,因此需要建立一种快速有效的方法用于贝母中异甾体生物碱的分析。本研究采用QuEChERS前处理技术萃取川贝母样品中贝母辛、贝母乙素及贝母甲素等异甾体生物碱,并结合液相色谱-串联质谱法(LC-MS/MS)进行分析。在QuEChERS优化条件下,取0.5g贝母样品,添加3mL含3%氨水的乙酸乙酯-水溶液(75∶25,V/V),再加入1g碳酸铵,振荡5min后,以4 000r/min离心5min,取1.8mL上清液,加入20mg硅酸镁及10mg无水硫酸镁,并以14 000r/min离心3min,氮气吹干后,用20%甲醇水溶液定量至1mL,采用LC-MS/MS法在正离子扫描模式下检测。结果表明:川贝母样品中贝母辛的线性范围为0.1~20μg/g,贝母乙素和贝母甲素的线性范围为0.05~10μg/g;线性相关系数(R2)大于0.992 3;检测限为0.005~0.03μg/g;日内与日间精密度的相对标准偏差介于1.1%~17.5%之间;回收率介于89.6%~97.0%之间。应用此方法检测真实样品,测得的异甾体生物碱含量中贝母辛为4.35μg/g,贝母乙素为0.92μg/g,贝母甲素为1.39μg/g。该方法具有前处理简便快速,样品和有机溶剂用量少等优点,可为其他贝母中生物碱的检测提供方法参考。
[Abstract]:Because of its effect of relieving cough and eliminating phlegm, Chuanbei is a kind of medicine with high economic value. Therefore, it is necessary to establish a rapid and effective method for the analysis of isosteroid alkaloids in Fritillaria japonica. In this study, isosteroidal alkaloids such as Beimuxin, Fritillatin B and Fritillatin A were extracted by QuEChERS pretreatment and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Under the optimized condition of QuEChERS, 0.5 g Fritillaria sample was added with 3mL containing 3% ammonia water (75: 25 V / V), then 1g ammonium carbonate was added. After oscillating 5min, the supernatant of 1.8mL was centrifuged for 5 min with 4 000r/min, and the supernatant of 1.8mL was obtained. 20mg magnesium silicate and 10mg anhydrous magnesium sulfate were added and centrifuged for 3 mins with 14 000r/min. After the nitrogen was blown dry, 20% methanol aqueous solution was used to quantify to 1 mL. The results were determined by LC-MS/MS method in positive ion scanning mode. The results showed that the linear range of berberine was 0. 1 渭 g / g, the linear range of Fritillatin B and Fritillatin was 0. 05 渭 g / g, the linear correlation coefficient (R2) was more than 0.992 3, the detection limit was 0. 005 ~ 0. 03 渭 g / g; The relative standard deviation between intra-day and inter-day precision was between 1.1% and 17.5%, and the recovery rate was between 89.6% and 97.0%. The content of isosteric alkaloids was 4.35 渭 g / g, 0.92 渭 g / g and 1.39 渭 g / g, respectively, and the results showed that the content of isosteroid alkaloids was 4.35 渭 g / g, 0.92 渭 g / g and 1.39 渭 g / g, respectively. This method has the advantages of simple and rapid pretreatment, low amount of samples and organic solvents, and can be used as a reference for the determination of alkaloids in other Fritillaria.
【作者单位】： 中兴大学化学系;朝阳科技大学银发产业管理系;
【分类号】：R284.1;O657.63
本文编号：2359607
[Abstract]:Because of its effect of relieving cough and eliminating phlegm, Chuanbei is a kind of medicine with high economic value. Therefore, it is necessary to establish a rapid and effective method for the analysis of isosteroid alkaloids in Fritillaria japonica. In this study, isosteroidal alkaloids such as Beimuxin, Fritillatin B and Fritillatin A were extracted by QuEChERS pretreatment and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Under the optimized condition of QuEChERS, 0.5 g Fritillaria sample was added with 3mL containing 3% ammonia water (75: 25 V / V), then 1g ammonium carbonate was added. After oscillating 5min, the supernatant of 1.8mL was centrifuged for 5 min with 4 000r/min, and the supernatant of 1.8mL was obtained. 20mg magnesium silicate and 10mg anhydrous magnesium sulfate were added and centrifuged for 3 mins with 14 000r/min. After the nitrogen was blown dry, 20% methanol aqueous solution was used to quantify to 1 mL. The results were determined by LC-MS/MS method in positive ion scanning mode. The results showed that the linear range of berberine was 0. 1 渭 g / g, the linear range of Fritillatin B and Fritillatin was 0. 05 渭 g / g, the linear correlation coefficient (R2) was more than 0.992 3, the detection limit was 0. 005 ~ 0. 03 渭 g / g; The relative standard deviation between intra-day and inter-day precision was between 1.1% and 17.5%, and the recovery rate was between 89.6% and 97.0%. The content of isosteric alkaloids was 4.35 渭 g / g, 0.92 渭 g / g and 1.39 渭 g / g, respectively, and the results showed that the content of isosteroid alkaloids was 4.35 渭 g / g, 0.92 渭 g / g and 1.39 渭 g / g, respectively. This method has the advantages of simple and rapid pretreatment, low amount of samples and organic solvents, and can be used as a reference for the determination of alkaloids in other Fritillaria.
【作者单位】： 中兴大学化学系;朝阳科技大学银发产业管理系;
【分类号】：R284.1;O657.63
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