Page 21 - Shimadzu Journal vol.2 Issue1

Posters from Recent Conferences

Poster 5 ASMS
These posters were presented at ASMS 2013 (June 9-13, 2013, Minneapolis) and
HPLC 2013 (June 16-20, Amsterdam). Click the title URLs to download Identification of antibacterial component from extract of Garcinia indica fruit rinds using LC/MS/MS
the posters of interest. Ionization of the sample for mass spectrometric analysis was carried out using the DUIS mode available in the LCMS-8040.
Here, both Electro-Spray Ionization (ESI) and Atmospheric Pressure Chemical Ionization (APCI) techniques are used
simultaneously; hence, polar to slightly mid-polar molecules can be analyzed in the same run. The LCMS-8040 has an
‘optimization of method’ feature in which the mass spectrometer selects the best product ion(s) and optimizes voltages and
collision energies for the precursor to product transition.

Poster 6 ASMS
Study of antibacterial activity of Essential Oil components obtained from pericarp of
Poster 1 ASMS Zanthoxylum rhetsa (Indian origin) using HS-GCMS
Development and Validation of LC/MS/MS Method with Ultra Small-Volume Injection for Initially, GCMS parameters were optimized by using direct liquid injection of EO. The individual components found in EO were
Quantitative Determination of Alprazolam in Human Plasma separated on Rtx-5Sil MS column. The n-alkane standard (C-7 to C-35) was injected for determination of LRIs of the components.
The FFNSC library with LRIs was used for qualitative confirmation. The headspace parameters for the EO in presence of complex
An LC/MS/MS method with an ultra small-volume injection for quantitative determination of alprazolam in human plasma has matrix like diluent, broth and culture were optimized.
been developed and validated using the Shimadzu LCMS-8080. The results indicate that the extra small injection volume
LC/MS/MS method did not change matrix effect behavior but greatly reduced contamination of the dirty plasma matrix to the
interface and ion optics. As such, the method is more robust and suitable for bioanalysis in heavily loaded research and service
laboratories. The method also makes it possible to handle a very small amount of available sample due to limited sample sources. Poster 7 ASMS
Structural Elucidation of N-glycans Originating From Ovarian Cancer Cells Using
High-Vacuum MALDI Mass Spectrometry
Poster 2 ASMS
MS2/MS3 was able to characterize with high detail the N-glycans of ovarian cancer cells and identify the different isobaric
Development of high speed CYP cocktail inhibition assay using UHPLC-MS/MS N-glycans occupying a single MS1 peak. Furthermore, with controlled high-energy fragmentation, MS3/MS4 was able to confirm
and characterize antenna modifications such as sialylation and fucosylation based on diagnostic ions.
A high-speed CYP cocktail inhibition assay using Nexera UHPLC combined with the LCMS-8080 has been developed. With the
conventional method using Shim-pack XR-ODS II columns (flow rate at 0.2 mL/min), all compounds eluted within 4.5 min (the
cycle time was 7 min). In contrast, the UHPLC method successfully reduced the cycle time to within 60 seconds without
sacrificing the data quality as the next sample was injected by overlapping with the last part of the previous analysis. Poster 8 ASMS
UHPLC-MS/MS improves the throughput 7 times compared with a conventional system.
Sensitive assay of free thyroid hormones by on line SPE-UHPLC-MS/MS in human plasma
Because of the low limit of quantification to attain, particular attention was given to extraction recovery and ion suppression.
To improve assay ruggedness and accuracy, deuterated analogues were used as internal standards. Mobile phase composition was
Poster 3 ASMS
optimized to generate the highest ionization efficiency. Both positive and negative ionization were investigated.
Characterization of products formed by forced degradation of Amlodipine Besylate using LC/MS/MS
Amlodipine was degraded under three different conditions and degradation products were studied. Structures were predicted
using fragmentation patterns. Initially, a chromatographic method was optimized using the gradient mode for Amlodipine Poster 9 ASMS
degradation products. The ESI MS/MS parameters were optimized, both for ionization source and collision energies, for the
observed degradation products. Depending on the degradation type, possible chemical reactions were predicted and Fragmentation Outcome Modelling: Prototype software for prediction of CID fragment ions
supported by fragmentation information from the LCMS-8080. for small molecule structures
The fragmentation of each molecule was unique with each fragment ion being a unique mass. For comparative purposes the total
number of fragment ions successfully predicted for each software package is expressed as a percentage of the total number of
Poster 4 ASMS experimental fragment ions. Results are presented as per the above order. Fragmentation Outcome Modeling was the only
application to successfully predict every fragment ion for each of the three examples given here.
Detecting Nucleoside Post Enzymatic Cleavage Modifications in RNA Using Fast Product Ion
Scanning Triple Quadrupole Mass Spectrometry
Scientists rely on LC-MS-MS for detection and quantitation of nucleosides. LC-MS-MS methods use MRM analysis for the Poster 10 ASMS
highest sensitivity and selectivity; however, these methods only detect analytes whose MRM transitions are known in
advance. Modified nucleosides are not easily identified by traditional MRM-based methods as many species share common Development and evaluation of Nano-ESI coupled to a triple quadrupole mass spectrometer
precursor and product ions. We developed LC-MS methods that utilize extremely fast product ion scanning for detection of for quantitative proteomics research
nucleosides obtained from commercial suppliers. Product ion spectra for each known nucleoside were acquired and inspected Digested BSA (Bovine Serum Albumin) was analyzed to optimize the conditions of the LC and the triple Q MS parameters. In
for common product ions. A mixture of modified nucleoside standards was analyzed as well.
summary, we improved the sensitivity of the triple Q MS by reducing the LC flow rate to nL/min. A few femtomoles of injected
peptides could be analyzed by nano-flow LC-MS. In this study, we developed and evaluated a novel quantitative system for
proteomics with the results suggesting that this system could be applied to shotgun proteomics.

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