Development of a high sensitivity bioanalytical method for alprazolam using ultra-perfor-mance liquid chromatography/tandem mass spectrometry

2010 ◽  
pp. n/a-n/a
Author(s):  
Joanne Mather ◽  
Paul D. Rainville ◽  
Warren B. Potts III ◽  
Norman W. Smith ◽  
Robert S. Plumb

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5721
Author(s):  
Han Young Eom ◽  
Seok-In Jang ◽  
Jong-Hwa Lee

Breast milk contains human milk oligosaccharides (HMOs), including sialyllactose (SL). SL is composed of sialic acid and lactose, and is divided into 3′-SL and 6′-SL according to the binding position. SL has immunoprotective effects against bacteria and viruses, and acts as a probiotic in the gastrointestinal tract. In this study, we developed a bioanalytical method for simultaneous analysis of 3′-SL and 6′-SL in liver and kidney tissues of Yucatan minipigs using liquid chromatography–tandem mass spectrometry (LC-MS/MS) under conditions optimized in our previous study. LC-MS/MS was performed using a hydrophilic interaction liquid chromatography (HILIC) column (50 mm × 2.1 mm, 3 μm) with a mobile phase consisting of 10 mM ammonium acetate in water (pH 4.5) and acetonitrile with gradient elution at a flow rate of 0.3 mL/min. A surrogate matrix method using water was applied for analysis of endogenous SL. The developed method was validated with regard to selectivity, linearity, precision, accuracy, the matrix effect, recovery, parallelism, dilution integrity, carryover, and stability according to the US Food and Drug Administration guidelines. We performed a tissue distribution study of minipigs, and analyzed liver and kidney tissues using the developed method to determine the tissue distribution of 3′-SL and 6′-SL. The tissue concentrations of 3′-SL and 6′-SL were readily measurable, suggesting that the method would be useful for evaluating the tissue distributions of these compounds in minipigs.



2020 ◽  
Vol 21 (15) ◽  
pp. 5449 ◽  
Author(s):  
Junhua Wang ◽  
Akhil Bhalla ◽  
Julie C. Ullman ◽  
Meng Fang ◽  
Ritesh Ravi ◽  
...  

We recently developed a blood–brain barrier (BBB)-penetrating enzyme transport vehicle (ETV) fused to the lysosomal enzyme iduronate 2-sulfatase (ETV:IDS) and demonstrated its ability to reduce glycosaminoglycan (GAG) accumulation in the brains of a mouse model of mucopolysaccharidosis (MPS) II. To accurately quantify GAGs, we developed a plate-based high-throughput enzymatic digestion assay coupled with liquid chromatography–tandem mass spectrometry (LC-MS/MS) to simultaneously measure heparan sulfate and dermatan sulfate derived disaccharides in tissue, cerebrospinal fluid (CSF) and individual cell populations isolated from mouse brain. The method offers ultra-high sensitivity enabling quantitation of specific GAG species in as low as 100,000 isolated neurons and a low volume of CSF. With an LOD at 3 ng/mL and LLOQs at 5–10 ng/mL, this method is at least five times more sensitive than previously reported approaches. Our analysis demonstrated that the accumulation of CSF and brain GAGs are in good correlation, supporting the potential use of CSF GAGs as a surrogate biomarker for brain GAGs. The bioanalytical method was qualified through the generation of standard curves in matrix for preclinical studies of CSF, demonstrating the feasibility of this assay for evaluating therapeutic effects of ETV:IDS in future studies and applications in a wide variety of MPS disorders.



2020 ◽  
Vol 1137 ◽  
pp. 121939
Author(s):  
Juliana Veloso Ferreira ◽  
Alysson Vinícius Braga ◽  
Renes de Resende Machado ◽  
Deborah Michel ◽  
Gerson Antônio Pianetti ◽  
...  


Sign in / Sign up

Export Citation Format

Share Document