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 >A rapid, simple, and high-throughput UPLC-MS/MS method for simultaneous determination of bioactive constituents in Salvia miltiorrhiza with positive/negative ionization switching
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A rapid, simple, and high-throughput UPLC-MS/MS method for simultaneous determination of bioactive constituents in Salvia miltiorrhiza with positive/negative ionization switching

机译:一种快速,简单,高通量的UPLC-MS / MS / MS方法,用于同时测定丹参中的生物活性成分,具有正/负离电离切换

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The dried root of Danshen (Salvia miltiorrhiza) is a Chinese medicine that has been used in traditional treatments for more than 2000 years in Asia. It has also been used to treat cardiovascular diseases for decades. The goal of this study was to develop a new, fast, and simple ultrahigh-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) analytical method for the analysis of phenolic acids and tanshinones in Danshen. The samples were separated on a Kinetex F5 column (2.1 x 100 mm, 1.7 mu m, pentafluorophenyl) using 78% acetonitrile with 0.1% formic acid as the mobile phase with iso-cratic elution while the flow rate was set at 0.45 mL/min. The analysis was performed in a Waters Xevo TQ mass spectrometer via multiple reaction monitoring (MRM) in polarity switching mode. The linearity values of the calibration curves of eight compounds were in the range from 3 to 3200 ng/mL (r(2) 0.99). Method validation was performed in terms of linearity, the relative standard deviations (RSDs) of the intra-day and inter-day, and it was found that precisions were within 15% and the accuracy ranged from 93% to 118%. The recovery was more than 87%. The limit of detection (LOD) and limit of quantification (LOQ) values of the eight analytes varied between 0.023 to 0.75 ng/mL and 0.375 to 1.5 ng/mL. respectively. This approach has the shortest analysis time for the separation of phenolic acids and tanshinones in Danshen using a UPLC core-shell column with F5 stationary phase. Meanwhile, this robust and high throughput method not only has a short run time (2 min) but also reduce the consumption of organic solvents. (C) 2018 Elsevier B.V. All rights reserved.
机译:Danshen(Salvia Miltiorrhiza)的干燥根是一种中药,在传统治疗中被用于亚洲超过2000年。几十年来,它也被用来治疗心血管疾病。本研究的目标是开发一种新的快速,简单的超高效液相色谱串联质谱(UPLC-MS / MS)分析方法,用于分析丹参的酚酸和丹参酮。使用78%乙腈在Kinetex F5柱(2.1×100mm,1.7μm,五氟苯基)上分离样品,其具有0.1%甲酸作为流动阶段,具有iso-Croatic洗脱,而流速设定为0.45ml / min 。通过极性切换模式的多次反应监测(MRM)在水中进行分析。 8个化合物的校准曲线的线性度值在3至3200ng / ml(R(2)& 0.99)的范围内。方法验证是在线性,日期内和日内的相对标准偏差(RSD)和白天的验证,并且发现精确在15%以内,精度范围为93%至118%。回收率超过87%。八个分析物的检测极限(LOD)和定量极限(LOQ)值在0.023至0.75ng / ml和0.375至1.5ng / ml之间变化。分别。这种方法具有使用F5固定相的U5核心壳柱分离Danshen中酚醛酸和坦啡酮的最短分析时间。同时,这种稳健且高通量的方法不仅具有短暂的运行时间(2分钟),而且还降低了有机溶剂的消耗。 (c)2018年elestvier b.v.保留所有权利。

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