Simultaneous quantification of individual intermediate steroids in silkworm ecdysone biosynthesis by liquid chromatography–tandem mass spectrometry with multiple reaction monitoring

2013 ◽  
Vol 915-916 ◽  
pp. 52-56 ◽  
Author(s):  
Juri Hikiba ◽  
Mari H. Ogihara ◽  
Masatoshi Iga ◽  
Kazuki Saito ◽  
Yoshinori Fujimoto ◽  
...  
2013 ◽  
Vol 742 ◽  
pp. 355-358
Author(s):  
Chao Jie Zhang ◽  
Geng Zhang ◽  
Lu Ting Chen ◽  
Qian Chen ◽  
Qi Zhou

This study focused on using liquid Chromatography Tandem Mass Spectrometry to detect N-Nitrosodimethylamine (NDMA) at trace concentrations in water. The water sample was preconcentrated by solid-phase extraction method. To find an elution which can obtain higher recovery, three reagents with different organic solvents were examined. After comparing the recoveries and the standard deviation of the elution, finally the dichloromethane was determined as the elution of the experiment. Then the concentrated sample was analyzed by a method combining SPE pretreatment and LC separation with tandem mass spectrometry using multiple reaction monitoring (MRM).


2018 ◽  
Vol 24 (3) ◽  
pp. 289-298
Author(s):  
Mahendra Shukla ◽  
Femi M Francis ◽  
Jawahar Lal

Conessine, a steroidal alkaloid obtained from the bark and seeds of the plant species of Apocynaceae family, elicits a histamine antagonistic action, selectively for the H3 histaminergic receptors. This alkaloid is used mainly for the treatment of dysentery and helminthic disorders. For the quantification of conessine in serum, a liquid chromatography–tandem mass spectrometry method was developed. Chromatographic separation was achieved on a Zorbax SB-CN column (100 × 4.6 mm, 3.5 µm), and a mobile phase consisting of 90% methanol in aqueous ammonium acetate buffer (pH 3.5) with 0.1% (v/v) formic acid at an isocratic flow rate of 0.6 ml/min at 40℃ provides efficiency in separation. A volume of 40 µl was injected each time and the run time for each sample was 5 min. Phenacetin (internal standard) was added to 50 µl of serum sample prior to liquid–liquid extraction using 3% isopropanol in n-hexane. The detection was performed on a 5500 QTRAP mass spectrometer by multiple reaction monitoring mode via electrospray ionization source. The multiple reaction monitoring of conessine and IS was m/ z 357.4 to m/ z 312.1 and m/ z 180.1 to m/ z 138.1, respectively. The method that showed selectivity and linearity in the range of 1–200 ng/ml was validated in terms of sensitivity, accuracy, precision and stability. The detection and quantitation limits were recognized at 0.1 and 1 ng/ml, respectively. The intra- and inter-day precision and accuracy fulfils the acceptance criteria. Applying the method to the pharmacokinetic studies in rats, conessine showed a peak serum concentration at 2 h post oral dose with a good bioavailability of 71.28 ± 4.65%.


Sign in / Sign up

Export Citation Format

Share Document