Page 21 - Shimadzu Journal vol.3 Issue3

Selection 9 Pharmaceutical, Life Science
Evaluation of a Novel Glass Vial Overcoming Adsorption Effect for Pharmaceutical Drugs
The majority of pharmaceutical drugs are still small molecule drugs. Adsorption onto consumables when in sample preparation is
regarded as a big issue. To overcome the adsorption effect, we developed and evaluated a novel glass vial “LabTotal vial” which is
highly inert to basic compounds and perfect for highly sensitive LC/MS analyses.

Selection 10 Pharmaceutical, Life Science
Flexible Automated Sample Preparation Workflows: Modified Automated Systems for Specific Immuno-MS and MS Workflows
The automation of sample preparation has become an increasingly important component for reproducible and operator-independent
experiments. The Perfinity Workstation has provided researchers established applications in affinity capture and digestion for targeted
proteomic workflows, utilizing specific affinity, IMER and reversed phase components coupled directly to a mass spectrometer. This work
outlines novel strategies that are being utilized for automated online and offline sample preparation to achieve these specific goals.

Selection 11 Pharmaceutical, Life Science
Highly Sensitive Quantitative Analysis of Amoxicillin and Clavulanic Acid from Plasma Using LC/MS/MS
Amoxicillin and clavulanic acid is a combination drug product in which amoxicillin is a β-lactam antibiotic, and clavulanic acid is a
β-lactamase inhibitor. In this combination, clavulanic acid acts by preventing the destruction of antibiotic amoxicillin which is used
to treat various bacterial infections. An LC-MS/MS method has been developed for highly sensitive quantitation of these molecules
from plasma using the Shimadzu LCMS-8040 triple quadrupole mass spectrometer.

Selection 12 Pharmaceutical, Life Science
Integration of Amino Acid, Acylcarnitine and Steroids Analysis in Single FIA/LC-MS/MS Platform
Traditionally, analysis of a steroid such as 17-hydroxyprogesterone is done by immunoassays but LC-MS/MS is an attractive
analytical alternative because it results in a reduction of false positives and a more accurate quantitative performance. The
requirements against steroid analysis by LC-MS/MS are getting more stringent. In this study, we present a strategy for performing
both AA/AC and steroids analysis within a single LC-MS/MS platform.
Selection 13 Pharmaceutical, Life Science
Non-convex Quasi-norm-based Normalization of MALDI-MS Imaging Data
We explore the use of non-convex quasi-norms as a normalization factor for MALDI-MS Imaging datasets. As a lower norm
parameter is used, results show less artefacts but less uniform normalization range. A trade-off value should be chosen. Results are
shown for decreasing concentrations of angiotensin peptide by itself and mixed with E.Coli (DH5 ) suspension.

Selection 14 Pharmaceutical, Life Science
N-terminal Charge-driven de novo Sequencing by using ASDF-incorporated Curved Field Reflectron
Fixing a strong charge at the N-terminus of a peptide has been reported to be an effective derivatization for de novo sequencing.
While giving high proton affinity at the N-terminus of a peptide facilitates the generation of a- and b-ions, it is impossible to
differentiate isobaric Ile/Leu residues. Side chain fragmentation generated by high-energy CID on MALDI-TOF/TOF has a potential to
overcome this issue. We report a discrimination of Ile/Leu and a capability of the assignment of Gln/Lys, applying a newly developed
MALDI-TOF/TOF, which has high resolution in MS/MS and a high energy CID at 20keV, for analysis of N-terminal derivatized peptides.

Selection 15 Pharmaceutical, Life Science
On-line Supercritical Fluid Extraction/Supercritical Fluid Chromatography:
A Novel Approach to the Cleaning Validation for pharmaceutical Manufacturing
Cleaning validation is necessary to establish the quality and safety of pharmaceutical drug products. Recently, HPLC has become
preferable because of the growing need for the individual analysis of products. Before the HPLC analysis, however, manual processes
such as a sample extraction and a sample condensation are required, which may affect the quality of results. Thus, we evaluated the
application of a novel on-line supercritical fluid extraction/chromatography system for the cleaning validation.
Selection 16 Pharmaceutical, Life Science
Quantification and Structural Characterization of Glycans and Glycopeptides by TQMS:
the Energy-resolved Oxonium Ion Monitoring (Erexim) Platform
We have previously reported on using a triple quadrupole mass spectrometer to reproducibly monitor glycan-derived low molecular weight
ions (oxonium ions) to acquire, within milliseconds, a profile of fragmentation patterns at a range of CID collision energies. This, which we
termed the energy-resolved oxonium ion monitoring (Erexim) profile, reflects the glycan structure in such a way that isobaric structures can
be clearly distinguished and assigned. Here we have developed new software to fully support Erexim data acquisition and analysis.

Selection 17 Pharmaceutical, Life Science
Structural Analysis of Isomeric Chemicals by Using High Resolution MS/MS on Curved Field Reflectron Incorporated with a Novel Focusing Technology
While resolution of MS has greatly improved, no matter how high it becomes, MS/MS remains essential to conduct analysis of
isomeric chemicals, and the analysis is thought to still be a significant task. Recently, we incorporated a new focusing technology
into the curved field reflectron, which enabled obtaining 10,000 resolution of MS/MS. We will apply the new curved field
reflectron toward ambiguous assignment and differentiation of isomeric chemicals.

Selection 18 Pharmaceutical, Life Science
Transfer of USP Normal Phase Method for the Analysis of Cortisone Acetate to the Nexera UC SFC System
The USP monographs are widely referenced to ensure the quality of drug substances. The USP monographs offer reliable and robust
methods. However, some of these methods, especially those using normal phase HPLC, require the use of harmful, even toxic
solvents. This application note shows an example of the analysis of cortisone acetate tablets according to the USP monograph.