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首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >LC-MS/MS determination of naringin, hesperidin and neohesperidin in rat serum after orally administrating the decoction of Bulpleurum falcatum L. and Fractus aurantii.
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LC-MS/MS determination of naringin, hesperidin and neohesperidin in rat serum after orally administrating the decoction of Bulpleurum falcatum L. and Fractus aurantii.

机译:口服青花菜和桔梗水煎液后,LC-MS / MS法测定大鼠血清中的柚皮苷,橙皮苷和新橙皮苷。

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To identify and quantify biologically active components in rat serum after orally administrating the decoction of Bulpleurum falcatum L. and Fractus aurantii, one of traditional Chinese medicines (TCMs), high-performance liquid chromatography (HPLC)-tandem mass spectrometry method was developed and validated. The HPLC separation was carried out on a Waters Nova Pak C(18) column using acetonitrile and water as mobile phase after the sample of rat serum was cleaned up with solid-phase extraction. Atmospheric pressure chemical ionization in the negative ion mode and selected reaction monitoring (SRM) method was developed to determine the active components. Three flavonoids of hesperidin, neohesperidin and naringin were identified in the serum by comparing their retention times and three independent SRM precursor/product ion transitions with those of corresponding reference standards. The concentrations of naringin, hesperidin and neohesperidin in rat serum determined by SRM measurement were 16.3, 11.9 and14.3 ng/ml, respectively, after orally administrating the decoction of B. falcatum L. and F. aurantii. This method was validated in terms of recovery, linearity, accuracy and precision (intra- and interday variation). The recoveries from spiked control samples were 93.0, 89.3 and 91.2% for hesperidin, neohesperidin and naringin, respectively. Linearity in rat serum was observed over the range of 2.0-50.0 ng/ml. Percent bias (accuracy) and precision were well within the acceptable range and the relative standard deviation (R.S.D.) of the measured rat serum samples was less than 10% (n=5).
机译:为了鉴定和定量口服青花菜和桔梗汤后大鼠血清中的生物活性成分,开发并验证了一种高效液相色谱法(HPLC)-串联质谱法作为中药(TCM)之一。 。在通过固相萃取净化大鼠血清样品后,在Waters Nova Pak C(18)色谱柱上使用乙腈和水作为流动相进行HPLC分离。开发了负离子模式下的大气压化学电离和选择的反应监测(SRM)方法来确定活性成分。通过比较其保留时间和三个独立的SRM前体/产物离子跃迁与相应参考标准品的保留时间,在血清中鉴定出了三种橙皮苷,新橙皮苷和柚皮苷。通过口服S. falcatum L.和A. aurantii煎汤后,通过SRM测定,大鼠血清中柚皮苷,橙皮苷和新橙皮苷的浓度分别为16.3、11.9和14.3 ng / ml。该方法在回收率,线性,准确性和精密度(日内和日间变化)方面得到了验证。从加标对照样品中提取的橙皮苷,新橙皮苷和柚皮苷的回收率分别为93.0%,89.3和91.2%。在2.0-50.0 ng / ml的范围内观察到大鼠血清中的线性。偏差百分比(准确性)和精密度均在可接受的范围内,并且所测大鼠血清样品的相对标准偏差(R.S.D.)小于10%(n = 5)。

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