【摘要】：川貝母具有止咳化痰之功效,是經(jīng)濟(jì)價(jià)值較高的藥品,因此市場(chǎng)上偶有將低價(jià)格貝母摻入其中的行為,因此需要建立一種快速有效的方法用于貝母中異甾體生物堿的分析。本研究采用QuEChERS前處理技術(shù)萃取川貝母樣品中貝母辛、貝母乙素及貝母甲素等異甾體生物堿,并結(jié)合液相色譜-串聯(lián)質(zhì)譜法(LC-MS/MS)進(jìn)行分析。在QuEChERS優(yōu)化條件下,取0.5g貝母樣品,添加3mL含3%氨水的乙酸乙酯-水溶液(75∶25,V/V),再加入1g碳酸銨,振蕩5min后,以4 000r/min離心5min,取1.8mL上清液,加入20mg硅酸鎂及10mg無(wú)水硫酸鎂,并以14 000r/min離心3min,氮?dú)獯蹈珊?用20%甲醇水溶液定量至1mL,采用LC-MS/MS法在正離子掃描模式下檢測(cè)。結(jié)果表明:川貝母樣品中貝母辛的線性范圍為0.1~20μg/g,貝母乙素和貝母甲素的線性范圍為0.05~10μg/g;線性相關(guān)系數(shù)(R2)大于0.992 3;檢測(cè)限為0.005~0.03μg/g;日內(nèi)與日間精密度的相對(duì)標(biāo)準(zhǔn)偏差介于1.1%~17.5%之間;回收率介于89.6%~97.0%之間。應(yīng)用此方法檢測(cè)真實(shí)樣品,測(cè)得的異甾體生物堿含量中貝母辛為4.35μg/g,貝母乙素為0.92μg/g,貝母甲素為1.39μg/g。該方法具有前處理簡(jiǎn)便快速,樣品和有機(jī)溶劑用量少等優(yōu)點(diǎn),可為其他貝母中生物堿的檢測(cè)提供方法參考。
[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.
【作者單位】： 中興大學(xué)化學(xué)系;朝陽(yáng)科技大學(xué)銀發(fā)產(chǎn)業(yè)管理系;
【分類號(hào)】：R284.1;O657.63

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