The EOHSI/NJDEP Analytical
Center is a state of the art facility designed to assist investigators
with difficult assays of biological and environmental contaminants or
their metabolites.
This facility has both inorganic
and organic analytical capabilities. The inductively coupled plasma/mass
spectrometers are the centerpieces of the inorganic analytical instrumentation.
They are the Fisons VG Plasma Quad II and the Fisons VG Plasma Quad
III. This device has the sensitivity to detect solution concentration
of metals down to pg/ml range. The ICP/MS has been used for trace metals
measurement in dust water soil and biologicals for the Childhood Lead
exposure Assessment and Reduction Study (CLEARS), the Treatment of Lead-exposed
Children (TLC), Jersey City Chromium project, and National Human Exposure
Assessment Study projects (NHEXAS).
Center personnel have interfaced
the ICP/MS to a Dionex DX 300 ion chromatograph which has allowed for
the speciation of metals at ultra-trace levels. This hyphenated technique
has been applied to the separation of the carcinogenic Cr(VI) from the
micro nutrient Cr(III) species. The speciation of chromium has allowed
investigators to enhance their research proposals. Since this method
was developed, it has been submitted for use in at least seven different
research proposals including the monitoring of remediated sites in chromium
contaminated areas in Hudson County. It has also been applied to the
examination of chromium in health food supplements.
Mercury has also been speciated
using the ICP/MS and ion chromatography technique. It can separate and
quantitate the various organic and inorganic mercury species down to
sub part per billion levels in solution. Solids, such as soil and lake
sediments samples, have been extracted and analyzed with this method.
As part of an NJ DEP funded research project for the development of
methods for quantifying ultra-trace levels of the different mercury
species in environmental samples mercury speciation has been used to
measure the different species of mercury in many of the lakes in New
Jersey.
Extraction of inorganic
contaminants from almost all matrices is accomplished by closed vessel
microwave digestion. The Analytical Center has a CEM 2100 D unit and
CEM MARS unit where both temperature and pressure in the vessels and
can be programmed for multi-step extraction procedures. The microwave
digestion techniques have been used for the digestion of chromium waste
contaminated soils as part of the Jersey City Chromium project. The
results obtained with the nitric acid microwave extraction method have
matched the hotplate HF digestion performed at Villanova University
on the same soil samples. This method has also been used for the digestion
of filter media used for dust wipe samples. The dust wipe sample and
digest procedures have been used in the TLC study, the CLEARS study
and the NHEXAS study. The mircowave has also been utilized in the extraction
of pesticides from from fat. This procedure is critical in the determination
of pesticides retained in the breast milk of nursing mothers.
The Analytical Center's
organic instrumentation is highlighted by the LCQ Classic Mass Spectrometer
interfaced with theWaters HPLC System, and the LCQ DECA Finigan Mass
Spectrometer interfaced with the Thermo Separation System.
Several methods have been
developed using the HPLC/ITMS including the analysis of catechins and
theoflavins. Essays for Tamoxifen (putative proginitor of hot flashes)
and 3-Methoxy-4hydroxyphenyl-glycol (MHPG) have been developed using
Solid Phase Extraction techniques. These were analyzed using and APCI
and ESI/MS/MS. A study of the metabolism of PhIP (2-amino-1-methyl-6-phenyllimidazo[4,5,b]pyridine
) using human liver or prostate microsomes utilizes the HPLC with mass
spectrometric detection using ESI positive mode with Selective Ion Monitoring
and MS/MS for PhIP and N-OH-PhIP in tandem with fluorescence detection.
Currently, the HPLC method to separate "-thujone (the active component
of absinthe) and its metabolites and their subsequent identification
by Mass Spectrometry is being developed.
The laboratory also has two Varian Saturn GC/IT Mass Spectrometers,
the 2000 and the 2200. This instrumentation is being extensively used
in to determine SVOC's including PAH's, PCB's, and pesticides in enviromental
samples. This research is currrentltly being funded by NJDEP and NIEHS
The Analytical Center possess
an OLIS RSM 1000 ultra-fast scanning UV/Vis absorbance spectrometer.
This device can be modified to operate in fluorescent mode and has a
stop-flow system for studying reactive chemical kinetics. The stop flow
system has been used to explore the reductive mechanisms of chromium
VI with cellular substituents. A cellular homogenate was used as one
of the reactants in the stop-flow mixing cell. End-on photomultiplier
tubes and a 1 kHz scan rate have allowed for measurement of millisecond
kinetics in turbid solutions. This instrument has also been used for
the measurement of chromaphores in microsomal solutions. Other Center
capabilities include purge and trap gas chromatography which is currently
configured for analysis of volatile organic carbons. It has also been
optimized for the separation of Methyl Tertiary Butyl Ether from Naphthalene.
The MTBE monitoring was part of a study that looked at the embryonic
mutations of freshwater fish caused by MTBE in conjunction with other
fuel additives. Center personnel also have access to GC/MS, flame Atomic
Absorption as well as conventional UV/Vis absorption spectroscopy.