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2
Experimental
Equipment
• The Agilent 1200 Infinity Series
LC Method Development Solution
comprised the following modules
with firmware revisions A.06.10 or
higher:
• Agilent 1290 Infinity Quaternary
Pump (G4204A)
• Agilent 1290 Infinity Autosampler
(G4226A)
• Agilent 1290 Infinity Thermostat
(G1330B)
• Two Agilent 1290 Infinity
Thermostatted Column
Compartments (G1316C) with built-
in high- and low-pressure column
switching valves, respectively
• Method development valve kit
(G4230B): high pressure with
method development capillary kit,
low dispersion, for short columns
• Agilent 1290 Infinity Diode Array
Detector (G4212A)
• Agilent 6140 Single Quadrupole
LC/MS System with multimode
source
• Several Agilent ZORBAX Rapid
Resolution High Throughput
(RRHT) 1.8-μm columns
• Agilent OpenLAB CDS
ChemStation Edition version
C.01.05 and Agilent MassHunter
Walkup software version C.01.00
can be performed on the Agilent 1200
Infinity Series LC Method Development
Solution and Agilent MassHunter Walkup
software. This LC system can be used
with up to eight columns of different
length and internal diameter. The
superuser can define different analytical
methods for the installed columns,
including appropriate equilibration
methods. The superuser can also define
projects for different user groups or single
users. Different permission levels can be
set for users and groups. Priorities can
be set; for example, reaction monitoring
samples can have highest priority and are
analyzed immediately. After completion of
the analysis, reports can be sent through
e-mail to the appropriate user.
In this Application Note, we used the
Agilent 1200 Infinity Series LC Method
Development Solution with attached
Agilent 6140 Single Quadrupole MS
in combination with the MassHunter
Walkup software for the following
laboratory environment:
• Three user groups need access to
the LC/MS system
• Four different projects are running
All groups have the following analytical
tasks:
• Reaction monitoring
• MS identification of the reaction
product
• Column scouting of reaction
mixtures to find the most suitable
column for preparative purification
• Purity control after preparative LC
Introduction
The main task of a chemical synthesis
laboratory is to generate new compounds
such as new drug compounds, new
pesticides, or new dyes that fulfill certain
prerequisites given by the governing
company. Typically, several attempts to
reach a desired structure are required
and often several modifications of
such a structure are desired as well.
The individual synthesis of compounds
involves reaction monitoring, control
of reaction products, and purity check
of compounds that were cleaned by
preparative LC. Traditionally, many of
these tasks have been done by thin
layer chromatography; however, with
rapid LC/MS instrumentation, results
can be achieved even faster, and most
importantly, with much more information
depth. That is the reason why more
companies make LC/MS systems
available to their chemists.
Recently, walk-up LC/MS systems are
used in these environments, which
provide easy access for inexperienced
users, analysis of the submitted
samples with predefined columns
and chromatographic methods, and
information about the results by, for
example, e-mail after completion of
the run. In many cases, these users
are unfamiliar with LC/MS systems.
Therefore, superusers take care of
the LC/MS system, providing the
chromatographic methods, keeping the
LC/MS system running and, in case of
errors, being able to restart the system.
Typically, several projects are done
in parallel. Therefore, different user
groups or single users need access to a
running LC system. Most important, the
different projects often require different
separation selectivity because of different
compound properties. All these tasks