scholarly journals Simultaneous Determination of Five Chromones of Radix Saposhnikoviae Extract in Rat Plasma by UPLC-MS/MS: Application to a Comparative Pharmacokinetic Study in Normal and Febrile Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Li Meng ◽  
Hui Gao ◽  
Bin Chen ◽  
Peng-peng Liu ◽  
Guo-shun Shan ◽  
...  

A rapid and sensitive quantitative analytical method was established for the simultaneous determination of five chromones (prim-O-glucosylcimifugin, cimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, 5-O-methylvisammiol, and sec-o-glucosylhamaudol) in the plasma of RS-treated rats for the first time using ultra performance liquid chromatography- (UPLC-) tandem mass spectrometry. The Waters Acquity UPLC BEH C18 (50 mm × 2.1 mm, 1.7 μm) was used as the chromatographic column, 0.1% formic acid water and 0.1% formic acid acetonitrile comprised the mobile phases, and all samples were determined under positive ion mode. The results showed that all analytes had good linearity (r>0.9902), between-day and within-day precisions less than 15%, accuracy between −5.50% and 5.53%, and extraction recovery between 88.26% and 97.65%. Both the matrix effect and stability met the requirements. This method was successfully applied for the comparative pharmacokinetics of five active components of RS in normal and febrile rats. The results showed that the pharmacokinetic behavior of RS extract significantly differed between the two types of rats.

2020 ◽  
Vol 15 (7) ◽  
pp. 1934578X2094011
Author(s):  
Safa M. Shams Eldin ◽  
Mohamed M. Radwan ◽  
Amira S. Wanas ◽  
Abdel-Azim M. Habib ◽  
Fahima F. Kassem ◽  
...  

In this study, an ultra-performance liquid chromatography (UPLC)/photodiode array method was developed for the simultaneous determination of trigonellan glucoside (1), isotrigonellan (2), and methoxy-isotrigonellan (3) in Trigonella stellata extract using an external standard method. The extract was prepared using a standardized method by maceration of the dried plant material in ethanol. The 3 isoflavans (1-3) were separated on an Acquity UPLC C18 column using gradient elution with a mobile phase consisting of 0.1% (v/v) formic acid aqueous solution and 0.1% (v/v) formic acid in acetonitrile, and ultraviolet detection. The method provides a linear correlation for all analytes over the investigated ranges with all correlation coefficients greater than 0.998. The validated lower limits of quantitation were 53, 127, and 5 μg/mL for isoflavans 1, 2, and 3, respectively. Intraday and interday precisions (percent relative SD [RSD%]) were less than 8.3% and accuracy (RE%) ranged from 90% to 100%. The method’s capability to remain unaffected by small, but deliberate variations in method parameters (method’s reliability during normal usage) described by the robustness showed RSD% less than 4.6% measured by varying 3 different parameters. The validated method was successfully applied to simultaneously determine the concentration of the 3 new isoflavans having anti-inflammatory and antidiabetic activities. The results revealed that the validated method can be used for quality control of herbal preparations containing these or similar isoflavans that are marketed for the prevention of inflammation and as antidiabetics.


2019 ◽  
Vol 15 (3) ◽  
pp. 231-242
Author(s):  
Ping Wang ◽  
Shenmeng Jiang ◽  
Yu Zhao ◽  
Shuo Sun ◽  
Xiaoli Wen ◽  
...  

Background: It is urgently needed to clarify the pharmacokinetic mechanism for the multibioactive constituents in Traditional Chinese Medicines for its clinical applications. A rapid, sensitive and reliable ultra-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of Danshensu, Ferulic acid, Astragaloside IV, Naringin, Neohesperidin and Puerarin after oral administration of Naoshuantong Granule using Carbamazepine as internal standard (IS). Methods: The plasma samples were pretreated by liquid-liquid extraction method using ethyl acetate after acidification, and separated on a Waters ACQUITY UPLC® BEH C18 column (50×2.1 mm, i.d., 1.7 µm) by gradient elution with a mobile phase composing of water (containing 0.1% formic acid) and acetonitrile at a flow rate of 0.2 mL/min. Multiple reaction monitoring (MRM) mode with both positive and negative ion mode was operated using an electrospray ionization (ESI) to detect the six compounds. Result: All calibration curves showed good linearity (r>0.99) over a wide concentration range. The intra- and inter-day precision (RSD%) was below 8.4% and the accuracy (RE%) ranged from 91.1% to 107.5%. The extraction recoveries of the six analytes and IS in the plasma were more than 77.9% and no severe matrix effect was observed. Conclusion: The fully validated method was successfully applied to the pharmacokinetics of Naoshuantong Granule.


Author(s):  
Maria Rincon Nigro ◽  
Jing Ma ◽  
Ololade Tosin Awosemo ◽  
Huan Xie ◽  
Omonike Arike Olaleye ◽  
...  

OJT007 is a methionine aminopeptidase 1 (MetAP1) inhibitor with potent anti-proliferative effects against Leishmania Major. In order to study its pharmacokinetics as a part of the drug development process, a sensitive, specific, and reproducible ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated. Voriconazole was used as the internal standard to generate standard curves ranging from 5 to 1000 ng/mL. The separation was achieved using a UPLC system equipped with an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) with 0.1% formic acid in acetonitrile and 0.1% formic acid in water as the mobile phase under gradient elution at a flow rate of 0.4 mL/min. The mass analysis was performed with a 4000 QTRAP® mass spectrometer using multiple-ion reaction monitoring (MRM) in the positive mode, with the transition of m/z 325 → m/z 205 for OJT007 and m/z 350 → m/z 101 for voriconazole. The intra- and inter-day precision and accuracy were within ±15%. The mean extraction recovery and the matrix effect were 95.1% and 7.96%, respectively, suggesting no significant matrix interfering with the quantification of the drug in rat plasma. This study was successfully used for the pharmacokinetic evaluation of OJT007 using the rat as an animal model.


2019 ◽  
Vol 2019 ◽  
pp. 1-12 ◽  
Author(s):  
Li Jiang ◽  
Yanling Xiong ◽  
Lanbin Yu ◽  
Yu Chen ◽  
Qiyun Zhang ◽  
...  

Huang-Lian Jie-Du decoction (HLJDD) has been used to treat cardiovascular and cerebrovascular disease for many years in China. Currently, the determination of effect components in HLJDD is focusing either on the formula or on the extract, while quantification of that in biological samples is scarce, especially simultaneous determination of multicomponent. In this paper, a rapid, specific, and sensitive ultra-high performance liquid chromatography-tandem mass spectrometry method was developed and fully validated for the simultaneous determination of seven main active constituents, i.e., baicalin, baicalein, wogonoside, wogonin, berberine, palmatine, jatrorrhizine in rat plasma. The method was also successfully applied to a quantitative study after oral administration of HLJDD at different doses of 1.5, 3, and 6 g/kg body weight to high fat-induced atherosclerosis rats. The analytes were detected by ESI source and multiple reactions monitoring (MRM) using positive scanning mode. The blood was collected from the abdominal aorta of rats at predetermined time and preprepared with icariin and tetrahydropalmatine as internal standards (IS). Sample preparation was achieved by protein precipitation (PPT). The validation parameters (linearity, sensitivity, intra-/interday precision and accuracy, extraction recovery, and matrix effect) were within acceptable ranges, and biological extracts were stable during the entire storing and preparing process. And the result of determination of HLJDD-containing plasma, baicalin, baicalein, wogonoside, and wogonin could be highly detected in a dose-dependent manner while berberine, jatrorrhizine, and palmatine were determined in a very low level and in a dose-independent mode. Thus, the established method was sensitive enough and successfully applied to the determination of seven effective components in plasma taken from 24 high fat-induced atherosclerosis rats after oral administration of three dosages of HLJDD.


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