Agilent ICP-MS Journal - Agilent Technologies
Agilent ICP-MS Journal - Agilent Technologies
Agilent ICP-MS Journal - Agilent Technologies
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<strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong><br />
January 2004 – Issue 18<br />
Inside this Issue<br />
2/3 Detecting "The New PCBs" using GC-<strong>ICP</strong>-<strong>MS</strong> - Challenges<br />
of PBDE Analysis<br />
4 User Profile: ExperTox Inc - Toxicology Laboratory, USA<br />
5 <strong>Agilent</strong> On-line Resources and Improved <strong>ICP</strong>-<strong>MS</strong> User Forum<br />
6 Phosphorus in Phosphorylated Deoxyribonucleotides using<br />
LC-<strong>ICP</strong>-<strong>MS</strong><br />
7 New Team Setup in the Americas<br />
8 Free Series of e-Seminars, Up & Coming Events, Welcome to<br />
New <strong>ICP</strong>-<strong>MS</strong> Users, New Literature
Detecting "New<br />
PCBs" using GC-<strong>ICP</strong>-<br />
<strong>MS</strong> - Challenges of<br />
PBDE Analysis<br />
Steve Wilbur and Emmett Soffey<br />
<strong>Agilent</strong> <strong>Technologies</strong>, Bellevue, WA, USA<br />
Introduction<br />
Brominated flame retardants and<br />
especially polybrominated diphenyl<br />
ethers (PBDEs) are under scrutiny<br />
around the world. PBDEs are widely<br />
used as flame retardants in plastics<br />
and are found in the plastics used<br />
in computers, construction materials,<br />
furniture and textiles. Structurally,<br />
they resemble PCBs, dioxins and<br />
furans, with the chlorines substituted<br />
by bromine. It is this similarity in<br />
structure coupled with recent data<br />
showing significant concentrations<br />
in the environment and human and<br />
animal tissues that has raised<br />
concern. A recent study in Sweden<br />
testing archived human breast milk<br />
showed levels 55 times higher in<br />
1997 than in 1972, with the average<br />
concentrations doubling every 5<br />
years. Further studies indicate that<br />
the US is far more contaminated<br />
than Sweden. For example, sewage<br />
sludge in the US contains 10-100<br />
times more PBDE than European<br />
sludge. While the global demand for<br />
PBDEs totaled 150 million pounds<br />
(68 million kg) in 1997, half of that<br />
was used by North American<br />
industries. Every day, the typical<br />
consumer comes in contact with<br />
dozens, if not hundreds of consumer<br />
goods that contain PBDEs. Since<br />
PBDEs are not covalently bound to<br />
the plastics into which they are<br />
incorporated, they are easily released<br />
into the environment. This can occur<br />
through incineration, leaching of<br />
materials in landfills, dust given off<br />
by degrading textiles and foam<br />
materials or even simple evaporation.<br />
Products containing these compounds<br />
typically contain from 5 to 20% of<br />
the product weight as PBDE.<br />
Because PBDEs are poorly soluble<br />
in water, but highly fat soluble, they<br />
are readily bioaccumulated in fatty<br />
tissues of animals and humans. Recent<br />
research on laboratory animals has<br />
shown that low level exposure to<br />
PBDEs can cause permanent<br />
neurological and developmental<br />
damage. Those most at risk are<br />
pregnant women, developing fetuses<br />
and young children. Already levels of<br />
PBDEs found in some mothers and<br />
fetuses are approaching levels known<br />
to impair learning and development<br />
in mice [1].<br />
Regulation<br />
As early as the mid 1980s to early<br />
1990s bans on the use of some PBDEs<br />
were proposed in Germany, Sweden<br />
and the Netherlands. In 1993, using<br />
its Dioxin Ordinance, Germany<br />
officially restricted the use of PBDEs<br />
because of the possibility of releasing<br />
dioxins when incinerated. In February<br />
2003, the EU announced a ban on<br />
two common PBDEs, Penta and<br />
Octa, in all products from August<br />
2004. The EU is also considering a<br />
ban on the use of Deca PBDE in<br />
electronics products by July 2006.<br />
Despite the much higher levels of<br />
PBDEs in North America, the US<br />
government has not imposed any<br />
regulations on their manufacture or<br />
use. Recently the State of California<br />
introduced legislation which would<br />
ban the use of several types of PBDEs<br />
by 2008. However, the California bill<br />
exempts the deca congener from<br />
the ban which is the most widely<br />
used type in electronic products.<br />
Several other states are considering<br />
similar legislation. Several Japanese<br />
electronic companies will be phasing<br />
PBDEs from their products and<br />
other countries and individual<br />
manufacturers are taking steps to<br />
eliminate their use of PBDEs.<br />
Structure<br />
The general structure of the PBDEs<br />
is given in Figure 1. There are ten<br />
possible sites for bromination; five<br />
on each ring. Similar to PCBs and<br />
dioxins, there are a large number of<br />
structural congeners depending on<br />
the number and location of bromine<br />
substitutions. In the case of PBDEs,<br />
there are 209 possible congeners, with<br />
the individual congeners named 1<br />
through 209. The decabromo congener<br />
is PBDE-209.<br />
Figure 1. General chemical structure of a<br />
polybrominated diphenyl ether<br />
Analytical Challenges<br />
Typically, PBDEs are analyzed and<br />
detected like PCBs or Dioxins using<br />
gas chromatography coupled to a<br />
halogen specific detector such as<br />
electron capture or to a mass<br />
spectrometer. However, unlike PCBs,<br />
PBDEs are much more difficult to<br />
separate and detect using<br />
chromatography. This is due to<br />
several differences between PCBs<br />
and PBDEs. PBDEs are high molecular<br />
weight, high boiling-point compounds<br />
which require high temperatures to<br />
elute from the GC column. However,<br />
unlike PCBs, which are very stable<br />
biphenyl compounds, the diphenyl<br />
ether structure makes PBDEs much<br />
more sensitive to degradation under<br />
high temperature GC conditions. In<br />
addition, the large number of bromines<br />
in the higher congeners places the<br />
molecular weight outside the range<br />
of some mass spectrometers.<br />
Furthermore, since bromine elicits<br />
a much lower response by electron<br />
capture than chlorine, the possibility<br />
of interferences from chlorinated<br />
compounds in some samples can be<br />
troublesome. Much work is ongoing<br />
to determine the optimum GC<br />
column dimensions and phase for<br />
PBDE analysis. At present, the<br />
best inertness for the sensitive 209<br />
congener has been shown to be a<br />
short, thin film 5 meter <strong>Agilent</strong><br />
DB-5 <strong>MS</strong> column [2]. Other columns<br />
tested show significant loss of the<br />
209 congener. However, this column<br />
is incapable of completely resolving<br />
all 209 congeners. Intensive research<br />
is ongoing at <strong>Agilent</strong> to determine<br />
the optimum chromatographic<br />
conditions for this analysis. In the<br />
meantime, only a few of the 209<br />
possible congeners are commonly<br />
used as flame retardants, so<br />
resolution of all 209 is not critical.<br />
The common commercial flame<br />
retardants are called Penta, Octa<br />
and Deca, though, for example, the<br />
Penta product is actually composed<br />
of 45% penta-BDE, 40% tetra and<br />
6% hexa congeners. Worldwide,<br />
the deca product, for which there<br />
is only one congener, is the most<br />
widely used, making up 83% by<br />
weight of the total usage. This<br />
congener is therefore the most<br />
important analytically. It is also<br />
the most difficult to measure.<br />
GC-<strong>ICP</strong>-<strong>MS</strong> Analysis<br />
Because the <strong>ICP</strong>-<strong>MS</strong> measures only<br />
the bromine, molecular weight is<br />
2 <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong> January 2004 - Issue 18 www.agilent.com/chem/icpms
not an issue for detection. Also,<br />
<strong>ICP</strong>-<strong>MS</strong> exhibits extremely high<br />
sensitivity and selectivity for bromine,<br />
eliminating possible interferences<br />
from other halogenated polyaromatic<br />
compounds. In this work [3], a mixture<br />
of 14 PBDE congeners ranging from<br />
#1 to #209 were analyzed by GC-<br />
<strong>ICP</strong>-<strong>MS</strong>. Operating conditions are<br />
given in Table 1. A chromatogram<br />
of the 10 ppb PBDE standard mix<br />
can be seen in Figure 2 with the<br />
identity of the peaks given in Table 2.<br />
GC<strong>Agilent</strong> 6890 with<br />
ALS and ChemStation<br />
software<br />
Column DB-XLB, 30m x 0.25mm<br />
LD x 0.1um (<strong>Agilent</strong><br />
part # 122-1231)<br />
Carrier Helium at 36cm/sec<br />
gas (1.5mL/min) at 100°C,<br />
constant flow mode<br />
Injector 320°C, splitless, 1uL<br />
Detector <strong>Agilent</strong> 7500cs <strong>ICP</strong>-<strong>MS</strong>,<br />
monitoring Br at m/z=81<br />
Table 1 Summary of GC-<strong>ICP</strong>-<strong>MS</strong> configuration<br />
Based on signal to noise measured<br />
in the 10 ppb standard (Figure 3),<br />
approximate detection limits are in<br />
the range of 100 ppt, which is<br />
comparable to those achievable by<br />
GC using a micro-ECD detector.<br />
However the <strong>ICP</strong>-<strong>MS</strong> "detector"<br />
exhibits superior linearity; does not<br />
suffer from non-analyte interferences;<br />
and can definitively identify<br />
brominated compounds. GC-<strong>ICP</strong>-<strong>MS</strong><br />
may well become the technique of<br />
choice for the trace level analysis<br />
of PBDEs in a variety of samples.<br />
Figure 3. Calibration curve (10ppb - 1 ppm) for<br />
PBDE-183 monitoring 79 Br<br />
www.agilent.com/chem/icpms<br />
Figure 2 GC-<strong>ICP</strong>-<strong>MS</strong> chromatogram of 10 ppb PBDE standard mix<br />
Peak Congener (2.5 mg/ml)<br />
1 2,2’,4-TriBDE (BDE-17)<br />
2 2,4’,4-TriBDE (BDE-28)<br />
3 2,3’,4’,6-TetraBDE (BDE-71)<br />
4 2,2’,4,4’-TetraBDE (BDE-47)<br />
5 2,3’,4,4’-TetraBDE (BDE-66)<br />
6 2,2’,4,4’6-PentaBDE (BDE-100)<br />
7 2,2’,4,4’5-PentaBDE (BDE-99)<br />
8 2,2’,3,4,4’-PentaBDE (BDE-85)<br />
9 2,2’,4,4’,5,6’-HexaBDE (BDE-154)<br />
10 2,2’,4,4’,5,5’-HexaBDE (BDE-153)<br />
11 2,2’,3,4,4’,5’-HexaBDE (BDE-138)<br />
12 2,2’,3,4,4’,5’,6-HeptaBDE (BDE-183)<br />
13 2,3,3’,4,4’,5,6-HeptaBDE (BDE-190)<br />
14 DecaBDE (BDE-209) (12,5 mg/ml)<br />
Table 2: PBDE peak identification<br />
References:<br />
1. S. Lunder and R. Sharp Tainted Catch, Environmental Working<br />
Group http://www.ewg.org<br />
2. J. Bjorklund, P Tollback and C Ostman, Poster Evaluation of the Gas<br />
Chromatographic Column System for the Determination of<br />
Polybrominated Dephenyl Ethers, Department of Analytical<br />
Chemistry, Stockholm University, Sweden<br />
3. E Kuhn, J. Ellis, S. Wilbur, T. Trainor, A. Gelbin GC Analysis of<br />
Polybrominated Flame Retardants Poster presented at Dioxin 2003<br />
Conference<br />
<strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong> January 2004 - Issue 18<br />
3
User Profile: ExperTox<br />
Inc. Specialists in<br />
Toxicology Testing<br />
Ernie Lykissa,<br />
ExperTox Inc, Texas, USA.<br />
Introduction<br />
ExperTox Inc. was established in<br />
1996 by Environmental Engineer<br />
Loretta M. Anderson and Forensic<br />
Toxicologist Dr. Ernest Lykissa, to<br />
address the increasing demand for<br />
toxicology studies from industry<br />
and State police departments.<br />
They equipped the laboratory with<br />
state-of-the-art instrumentation to<br />
tackle a varied workload including<br />
requests from individuals, industry<br />
or the police for certified analysis<br />
of biological specimens to include<br />
hair, urine blood, tissue and saliva.<br />
The most common request is to test<br />
for any evidence of poisoning or<br />
exposure to certain organics or heavy<br />
metals. ExperTox also conduct a full<br />
range of employment testing, including<br />
drug testing for non-prescribed<br />
narcotics. They will also establish<br />
baseline levels of residual metals<br />
present in contractors and employees<br />
working in heavy industry who may<br />
be exposed to toxic substances in the<br />
course of their work. Other examples<br />
of work undertaken include:<br />
• Analysis of food and nutritional<br />
supplements<br />
• Analysis of date rape drugs,<br />
drugs of abuse and steroids<br />
• Expert witness testimony in<br />
family, civil and criminal courts<br />
A team of chemists, biologists,<br />
medical technicians and toxicologists<br />
use a full range of analytical<br />
equipment, including <strong>ICP</strong>-<strong>MS</strong>, GC-<br />
<strong>MS</strong>, LC-<strong>MS</strong>, EIA (electrothermal<br />
atomization), HPLC and microscopic<br />
analysis, to carry out a full evaluation<br />
and report for each project.<br />
The Role of <strong>ICP</strong>-<strong>MS</strong><br />
ExperTox Inc were one of the first<br />
laboratories in the US to endorse<br />
the <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong>. They purchased<br />
a 4500 in 1996 and one of the first<br />
7500 systems in 2000. With previous<br />
experience as the head of a drug<br />
testing department for a large<br />
pharmaceutical company, Dr Lykissa<br />
was confident that all the heavy metal<br />
determinations could be handled<br />
directly by <strong>ICP</strong>-<strong>MS</strong> without the need<br />
to invest in additional techniques<br />
like Graphite Furnace Atomic<br />
Absorption (GFAAS). "GFAAS is old<br />
technology, <strong>ICP</strong>-<strong>MS</strong> is a much more<br />
powerful and productive technique<br />
that suits our needs perfectly,"<br />
commented Dr Lykissa.<br />
Analysis of Clinical Samples<br />
Primarily, <strong>ICP</strong>-<strong>MS</strong> is used to<br />
determine heavy metals such as lead,<br />
cadmium, chromium, cobalt, mercury<br />
and platinum. First, all samples of<br />
urine, blood, and other tissues are<br />
hydrolyzed in 5 % HNO3. Gold is<br />
added (10 ug/L) to stabilize any<br />
mercury present in the specimens.<br />
The toxic concentration of most<br />
heavy metals is in the high ppb (ug/L)<br />
range. Anything higher than that is<br />
indicative of an acute exposure and<br />
would require further investigation.<br />
The samples are then analyzed using<br />
the 7500a <strong>ICP</strong>-<strong>MS</strong> fitted with a High<br />
Solids (Babington type) nebulizer<br />
and standard quartz spray chamber.<br />
The instrument is optimized using<br />
a solution containing Li, Y, Ce and<br />
Tl (10ppb) for standard low-oxide/low<br />
interference levels (~0.3% CeO/Ce)<br />
while maintaining high sensitivity<br />
across the mass range. Typical<br />
instrumental conditions are displayed<br />
in Table 1.<br />
Parameter Value<br />
Forward Power 1200 W<br />
Plasma Gas Flow 15.0 L min-1<br />
Auxiliary Gas Flow 1.0 L min-1<br />
Nebulizer Gas Flow 1.2 L min-1<br />
Sampling Depth 0.5 mm<br />
Integration time 3 sec<br />
No. replicates per 3<br />
analysis<br />
Table 1 Instrumental conditions<br />
Results and Discussion<br />
For quantitative results, the<br />
instrument is calibrated using a<br />
mixed concentration multielement<br />
solution containing Ag, As, Cd, Co,<br />
Cr, Ni, Pb, Se, Al, Cu. Hg is calibrated<br />
with its own standard. Analysts<br />
also employ commercial quality<br />
controls for whole blood and urine<br />
that contain the above metals in<br />
normal and elevated concentrations.<br />
Table 1 shows 7500a data obtained<br />
on five different days compared to<br />
reference values obtained from preassayed<br />
blood reference standards.<br />
Element Ref <strong>ICP</strong>-<strong>MS</strong> data<br />
value<br />
ng/mL<br />
over 5 days<br />
As 88 88.2, 83.5, 85.3, 88.9,<br />
88.2<br />
Cd 13 12.4, 12.8, 12.5, 12.8,<br />
12.8<br />
Cr 60 54.6, 58.5, 59,2, 55.6,<br />
56.7<br />
Pb 57 57.2, 57.0, 57.7, 56.8,<br />
57,2<br />
Hg 43 42.4,42.8,44.2,43.5,<br />
43.6<br />
Se 570 562 , 573, 576, 568,<br />
567<br />
Table 1. <strong>ICP</strong>-<strong>MS</strong> control performance data over<br />
5 different days<br />
Case Study Example<br />
ExperTox worked on the case of a<br />
prominent cardiologist who suspected<br />
an estranged girlfriend of poisoning<br />
him. Tests determined the arsenic<br />
level in his urine to be 850 ug/L -<br />
way in excess of normal levels of<br />
20 ug/L and toxic levels of 100<br />
ug/L. Could this be a case of foul<br />
play? Upon close examination and<br />
testing of his house, CCA (copper,<br />
chromium, arsenic salt) treated<br />
wood and insulation material were<br />
discovered in the attic. Recent<br />
flooding in the area had created<br />
damp conditions for mold to thrive.<br />
The mold had absorbed considerable<br />
amounts of the toxic CCA which was<br />
spread throughout the house after<br />
gaining access to the air-conditioning<br />
ducts. The physician abandoned his<br />
house immediately and his urinary<br />
arsenic levels returned to normal,<br />
in a period of 30 days! Case solved.<br />
For more information on Expertox<br />
visit: http://www.expertox.com<br />
7500 Makes TV Debut!<br />
A 7500 <strong>ICP</strong>-<strong>MS</strong> and other <strong>Agilent</strong> equipment,<br />
including a 5973 GC-<strong>MS</strong>, can be seen in the<br />
current series of the US TV show Crime Scene<br />
Investigation (CSI). CSI is a very popular<br />
American primetime series that features a<br />
team of forensic investigators trained to solve<br />
crimes by careful analysis of the crime scene<br />
evidence. Equipping the forensics lab with<br />
state-of-the-art instrumentation adds to the<br />
credibility of the show - if not to its popularity.<br />
4 <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong> January 2004 - Issue 18 www.agilent.com/chem/icpms
<strong>Agilent</strong> On-line<br />
Resources at<br />
Your Fingertips<br />
Karen Morton, <strong>Agilent</strong> UK<br />
Have you seen the latest video<br />
release on the <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> web<br />
site? Follow the link from<br />
www.agilent.com/chem/icpms and<br />
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There are now more than 300<br />
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<strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong> January 2004 - Issue 18<br />
5
Phosphorus in<br />
Phosphorylated<br />
Deoxyribonucleotides<br />
using LC-<strong>ICP</strong>-<strong>MS</strong><br />
Daniel Profrock, Peter Leonhard<br />
and Andreas Prange, GKSS Research<br />
Centre Geesthacht, Germany.<br />
Introduction<br />
Phosphorus plays an important role in<br />
cell biology for protein phosphorylation,<br />
energy storage and transport at<br />
the cellular level or as one essential<br />
part of the ribose-deoxyribose<br />
phosphorus backbone in the RNA<br />
or DNA chain [1]. The measurement<br />
of phosphorus would provide<br />
information about the phosphorylation<br />
state of a protein, which, in turn, has<br />
a significant effect on different<br />
metabolic pathways. Measuring<br />
phosphorus can also be used for the<br />
detection and quantification of RNA<br />
or DNA due to the fixed stoichiometry<br />
of this element in the above mentioned<br />
macro molecules.<br />
<strong>ICP</strong>-<strong>MS</strong> represents a highly sensitive<br />
technique for the determination of<br />
phosphorus in biological samples.<br />
Moreover, the <strong>Agilent</strong> 7500c Octopole<br />
Reaction System (ORS) <strong>ICP</strong>-<strong>MS</strong><br />
overcomes the limitation of<br />
conventional systems by removing<br />
the interferences caused by<br />
polyatomic ions ( 14 N 16 O 1 H, 15 N 16 O)<br />
on mass 31 P [2].<br />
<strong>ICP</strong>-<strong>MS</strong> Experiments<br />
The 7500c was optimized to minimize<br />
the background of the interfering<br />
ions on phosphorus while maintaining<br />
good overall sensitivity.<br />
Instrumental detection limits for<br />
the simultaneous determination of<br />
phosphorus and other trace elements<br />
in an aqueous solution were<br />
calculated.<br />
Detection limits down to 125 ng/L<br />
were achieved for phosphorus and<br />
from 18 ng/L ( 55Mn) up to 49 ng/L<br />
( 54Fe) for other trace elements<br />
measured simultaneously. The<br />
detection limits for all elements<br />
measured are summarized in Table 1.<br />
Isotope (mass) Detection limit<br />
(ng/L)<br />
P (31) 125<br />
Cr (52) 21<br />
Mn (55) 18<br />
Fe (54) 49<br />
Ni (58) 26<br />
Co (59) 19<br />
Cu (63) 25<br />
Zn (66) 37<br />
Cd (114) 32<br />
Pb (208) 24<br />
Table 1 Detection limits for phosphorus and some<br />
selected simultaneously detected trace elements<br />
in an aqueous, acidified solution, estimated<br />
according to the method outlined in ref. 3.<br />
HPLC-<strong>ICP</strong>-<strong>MS</strong> Experiments<br />
Using UV detection at 254.4nm,<br />
method optimization was undertaken<br />
with a mixture of dUMP, dAMP,<br />
dGMP, dCMP and cTMP. Based on<br />
the results, a 15 mmol L21, pH 5.8<br />
ammonium acetate buffer and 2.5%<br />
methanol (v/v) were used for all<br />
further experiments. The setup<br />
provides baseline separation of the<br />
five investigated compounds in ca. 12<br />
min.<br />
Figure 1a shows a chromatogram of<br />
the element specific determination<br />
of phosphorus in deoxynucleotides<br />
obtained by HPLC-ORS-<strong>ICP</strong>-<strong>MS</strong>.<br />
Single compound samples were used<br />
for peak assignment. The chromatogram<br />
shows one phosphorus- containing<br />
(but not UV active) peak, which<br />
remains unidentified. Detection<br />
limits based on the compound and<br />
on phosphorus were calculated for<br />
each dNMP - see Table 2. An aliquot of<br />
enzymatically digested calf thymus<br />
DNA sample was also separated<br />
under optimized HPLC conditions -<br />
see Figure 1b. The four nucleotides<br />
were baseline separated. Single<br />
compound samples and mixtures of<br />
commercially available deoxynucleotides<br />
were used for peak identification.<br />
Figure 1 Separation and element<br />
specific detection of calf thymus<br />
DNA digested with nuclease P1<br />
analyzed with HPLC-ORS-<strong>ICP</strong>-<strong>MS</strong>.<br />
(a) Mixture of dAMP, dCMP, dGMP<br />
and dTMP (100 mg/L of each compound)<br />
measured on the mass of 31<br />
P for comparison of the retention<br />
times. (b) Enzymatic digest of calf<br />
thymus DNA with nuclease P1<br />
measured on the mass of 31 P.<br />
J. Anal. At. Spectrom., 2003, 18, 708-713 -<br />
Reproduced by permission of The Royal<br />
Society of Chemistry<br />
The four peaks in the chromatogram<br />
could be clearly assigned to dAMP,<br />
dGMP, dCMP and dTMP by comparison<br />
of the retention times. New unknown<br />
peaks were also found during<br />
chromatographic separation of<br />
enzymatically digested DNA samples<br />
which could not be identified by<br />
comparison of the retention times.<br />
Species DL species DL of P DL of P<br />
(ug/L) in dNMP<br />
(ug/L)<br />
absolute (pg)<br />
dAMP 48 5 50<br />
dGMP 56 6 60<br />
dCMP 42 4 40<br />
dTMP 34 3 30<br />
Table 2. Detection limit for phosphorus in<br />
monophosphorylated deoxynucleotides obtained<br />
with HPLC-ORS-<strong>ICP</strong>-<strong>MS</strong><br />
Conclusions<br />
Using the <strong>Agilent</strong> 7500c ORS-<strong>ICP</strong>-<strong>MS</strong><br />
as a sophisticated detector for HPLC<br />
has proved to be a suitable technique<br />
for the separation and element specific<br />
determination of phosphorylated<br />
deoxynucleotides via the phosphorus<br />
located in the sugar backbone of each<br />
nucleotide. Polyatomic ions formed<br />
in the plasma and the interface region<br />
of the <strong>ICP</strong>-<strong>MS</strong> that interfere with the<br />
determination of P at mass 31 were<br />
minimized by the addition of helium<br />
to the collision cell, allowing detection<br />
limits down to 3 ug/L for dTMP.<br />
Furthermore, used as a standalone<br />
<strong>ICP</strong>-<strong>MS</strong>, the <strong>Agilent</strong> 7500c can be used<br />
for the simultaneous determination of<br />
phosphorus and other trace elements<br />
in acidified aqueous solutions down<br />
to the low-ppt level.<br />
References<br />
1 G. Loffler and P. E. Petrides, Biochemie<br />
und Pathobiochemie, Springer, 1998, pp.<br />
23-30.<br />
2 N. Yamada, J. Takahashi and K. Sakata, J.<br />
Anal. At. Spectrom., 2002, 17, 1213-1222.<br />
3 D. R. Bandura, V. I. Baranov and S. C.<br />
Tanner, Anal. Chem., 2002, 74, 1497-1502.<br />
6 <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong> January 2004 - Issue 18 www.agilent.com/chem/icpms
New <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong><br />
Team in North<br />
America<br />
Karen Morton, <strong>Agilent</strong> UK<br />
karen@agilenticpms.com<br />
<strong>Agilent</strong> is investing heavily in<br />
technical support for its <strong>ICP</strong>-<strong>MS</strong><br />
users in North America. Don Potter<br />
has taken over management of the<br />
technical sales and applications<br />
support in the Americas. In addition<br />
to his existing position as <strong>ICP</strong>-<strong>MS</strong><br />
Program Manager in Europe, Don<br />
is now also <strong>ICP</strong>-<strong>MS</strong> Program Manager<br />
for the Americas (Chris Tye performs<br />
a similar role for <strong>Agilent</strong> covering<br />
Japan and Asia/Pacific region).<br />
Don brings 20 years of experience<br />
in <strong>ICP</strong>-<strong>MS</strong> (11 years with <strong>Agilent</strong>)<br />
to the Americas team, and some<br />
new team members to increase the<br />
level of our support.<br />
Technical sales support is now<br />
handled by two product specialists:<br />
Brenda Watson, based in Houston,<br />
TX, has been with <strong>Agilent</strong> for 15<br />
years, formerly working in R&D,<br />
and as a field engineer. Brenda is<br />
responsible for the Western US<br />
states plus TX and LA. We also<br />
welcome back Abe Gutierrez<br />
(Weston, FL), who is responsible<br />
for the Eastern US and Canada.<br />
Abe originally spent 6 years with<br />
<strong>Agilent</strong> as an <strong>ICP</strong>-<strong>MS</strong> applications<br />
chemist and product specialist,<br />
and brings a wealth of experience<br />
to the team. We are also excited to<br />
announce the addition of Lisa<br />
Clark to our team, who will be<br />
working with Abe in a technical<br />
support role. Lisa joins us from<br />
Ashland Chemicals where she was<br />
an inorganic lab manager. While at<br />
Ashland, Lisa set up a state of the<br />
art semiconductor chemicals clean<br />
lab. We will be offering Lisa's<br />
expertise on a consultancy basis to<br />
advise on the set up of a trace<br />
metals analysis lab or laboratory<br />
clean room design.<br />
We have also made significant<br />
additions to our applications support<br />
team. Chris Scanlon (Livonia, MI)<br />
who has 10 years experience in<br />
<strong>ICP</strong>-<strong>MS</strong> as a product specialist with<br />
<strong>Agilent</strong> moves to applications<br />
support, joining Emmett Soffey<br />
(Bellevue, WA), also with 10 years<br />
<strong>ICP</strong>-<strong>MS</strong> experience at <strong>Agilent</strong>.<br />
Emmett, like Chris, also has many<br />
www.agilent.com/chem/icpms<br />
The <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> Team at the Winter Plasma Conference, January 2004, Ft. Lauderdale, USA<br />
years experience with GC and LC<br />
and supports our fast expanding<br />
GC-<strong>ICP</strong>-<strong>MS</strong> and LC-<strong>ICP</strong>-<strong>MS</strong> userbase.<br />
Due to the increased demand for<br />
on-site <strong>ICP</strong>-<strong>MS</strong> consulting and<br />
classroom training, we have also<br />
formed an applications consultant<br />
team. We currently have three fully<br />
trained consultants whom we<br />
contract with to provide on-site<br />
training. Dr. Johan Schijf of the<br />
University of S. Florida has been<br />
delivering our training classes at our<br />
Wilmington, DE facility for the past<br />
two years, and we welcome Dr Tom<br />
Rettberg, formerly VG/Thermo<br />
<strong>ICP</strong>-<strong>MS</strong> manager, into the team as<br />
applications consultant. Tom has over<br />
15 years experience in <strong>ICP</strong>-<strong>MS</strong> and<br />
is very well known in the industry.<br />
We also welcome back former <strong>Agilent</strong><br />
application chemist Mike Radle as<br />
a consultant for semiconductor<br />
applications.<br />
In addition to this very strong team,<br />
we also have Steve Wilbur (Bellevue,<br />
WA), worldwide environmental<br />
<strong>ICP</strong>-<strong>MS</strong> specialist based in the US.<br />
Steve is one of the leading authorities<br />
on GC-<strong>ICP</strong>-<strong>MS</strong>, having co-developed<br />
the <strong>Agilent</strong> GC interface and written<br />
extensively on the subject.<br />
For hardware support, we now have<br />
22 factory trained <strong>ICP</strong>-<strong>MS</strong> hardware<br />
engineers in N. America and we<br />
will add more as needs arise. This<br />
team is supported and trained by<br />
<strong>ICP</strong>-<strong>MS</strong> product support engineer<br />
Ron Sanderson (Dayton, OH) to<br />
ensure our <strong>ICP</strong>-<strong>MS</strong> support is<br />
maintained at the highest standards<br />
available in the industry.<br />
<strong>Agilent</strong> is absolutely committed to<br />
supporting its N. American <strong>ICP</strong>-<strong>MS</strong><br />
customers and with this new team<br />
now in place we are confident we<br />
are delivering the highest quality<br />
support for our <strong>ICP</strong>-<strong>MS</strong> customers.<br />
We'll bring you news of additions<br />
to our <strong>ICP</strong>-<strong>MS</strong> support teams in<br />
Latin America, Europe and<br />
Asia/Pacific in future issues of the<br />
<strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong>.<br />
Some contact e-mail addresses are<br />
given below:<br />
Don Potter<br />
don_potter@agilent.com<br />
Chris Scanlon:<br />
chris_scanlon@agilent.com<br />
Abe Gutierrez:<br />
abe@agilenticpms.com<br />
Emmett Soffey:<br />
emmett_soffey@agilent.com<br />
Brenda Watson:<br />
brenda_watson@agilent.com<br />
Tom Rettberg:<br />
trett@agilenticpms.com<br />
Dr. Johan Schijf:<br />
johan@agilenticpms.com<br />
Lisa Clark:<br />
lisa@agilenticpms.com<br />
Mike Radle:<br />
mike@agilenticpms.com<br />
<strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong> January 2004 - Issue 18<br />
7
<strong>ICP</strong>-<strong>MS</strong> e-Seminar<br />
Series 2004<br />
Join our free 60 minute e-seminars<br />
designed to help you get the most<br />
from your <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> from the<br />
comfort of your office.<br />
Applying Reaction Cell <strong>ICP</strong>-<strong>MS</strong> to<br />
Routine Multielement Analysis<br />
Ed McCurdy (Manchester, UK)<br />
February 18 - 2pm UK, 3pm<br />
Europe, 9am EST, 6am PST<br />
February 25 - 2 pm EST, 11am PST<br />
Environmental Analysis:<br />
A Comparison of Cell and Non-cell<br />
<strong>ICP</strong>-<strong>MS</strong><br />
Emmett Soffey (Bellevue, WA, USA)<br />
March 16 - 2pm UK, 3pm Europe,<br />
9am EST, 6am PST<br />
March 23 - 2 pm EST, 11am PST<br />
Developments in Speciation<br />
Measurement with <strong>ICP</strong>-<strong>MS</strong> as a<br />
Detector<br />
Steve Wilbur (Bellevue, WA, USA)<br />
March 18 - 2pm UK, 3pm Europe,<br />
9am EST, 6am PST<br />
March 25 - 2 pm EST, 11am PST<br />
Semiconductor Applications of<br />
Octopole Reaction Cell <strong>ICP</strong>-<strong>MS</strong><br />
Abe Gutierrez (Miami, FL, USA)<br />
March 24 - 2pm UK, 3pm Europe,<br />
9am EST, 6am PST<br />
March 31 - 2 pm EST, 11am PST<br />
Reaction Cell <strong>ICP</strong>-<strong>MS</strong> for<br />
Environmental Metals Analysis<br />
Steve Wilbur (Bellevue, WA, USA)<br />
April 8 - 4pm UK, 5pm Europe,<br />
11am EST, 8am PST<br />
To register visit<br />
www.agilent.com/chem/icpms<br />
and click on the e-Seminar<br />
Highlight for more information.<br />
Toll-free or local rate phone numbers<br />
are now available in the following<br />
countries: Austria, Belgium, Canada,<br />
Denmark, France, Germany, Ireland,<br />
Italy, Netherlands, Norway, Spain,<br />
Sweden, Switzerland, UK and USA.<br />
Events<br />
Pittcon<br />
March 7-12 2004, Chicago, USA<br />
http://www.pittcon.org/<br />
Forum Labo<br />
March 23-26 2004, Paris, France<br />
http://www.forumlabo.com<br />
This information is subject to change<br />
without notice<br />
© <strong>Agilent</strong> <strong>Technologies</strong>, Inc. 2004<br />
Printed in the U.S.A. January 27, 2004<br />
5989-0588EN<br />
New Members of the <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> Club<br />
A very warm welcome to the following companies and institutions<br />
that have recently added an <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> to their analytical facilities.<br />
• North Creek Analytical 5, USA • Texas DOH, USA • Westinghouse<br />
Savannah River 2, USA • UCLA, USA • USDA Alameda, USA • Ministerio<br />
de Salud, Panama • USDA Riverside, USA • Batelle 2, USA • GLA Labs,<br />
USA • BSI Inspectorate, USA • Univ of Delaware, USA • Chiron, USA •<br />
Georgia EPA, USA • Instituto Mexicano del Petróleo, Mexico • Jamaica<br />
Bureau of Standards, Jamaica • CEPIS, Peru • Policia de Investigaciones<br />
de Chile, Chile • ETH Zurich, Switzerland •ARPA Perugia, Italy • Agri<br />
Paradigma, Italy • STUA Lunebourg, Germany • Paks, Hungary • Uni<br />
Graz 4, Austria • Labor Dr Wessling 3, France •Labor Dr Wessling 2,<br />
Germany • Uni Essen 2, Germany • Uni Seville, Spain • Special Metals,<br />
UK • AES Howden, UK • LGC 2, UK • ATU, Germany • Inst of Food<br />
Research, UK • ASM Terni, Italy • Amdel Industrial & Environmental,<br />
Australasia • Chinese University HK, Hong Kong • KT & G Central<br />
Research Institute, Korea • Nongshim Anyang Factory, Korea • Ministry<br />
of Agriculture, PR China • Qingdao Ocean University, PR China •<br />
Shanghai Jintong University, PR China • UMC (Hsinchu) 2, Taiwan, •<br />
UMC (Hsinchu) 3, Taiwan<br />
Easier to Use <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> User Forum<br />
The <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> User Forum is now much easier to use and more<br />
intuitive thanks to its new and more powerful platform. For those not<br />
familiar with the User Forum, it's an on-line tool designed strictly for<br />
<strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> users wishing to share information relating to their <strong>ICP</strong>-<strong>MS</strong>.<br />
Questions can be applications, hardware, software, model/accessory,<br />
support specific or anything you like! New features include:<br />
• Identify new postings and discussions of interest to you.<br />
• Elect to "subscribe" to receive e-mail notification of new postings.<br />
• Search previous postings for key words or phrases using the basic or<br />
advanced search facility.<br />
• Rate your interest in the discussion, and even choose to ignore a topic<br />
that isn't relevant to you.<br />
Why not take a look?<br />
To access the <strong>ICP</strong>-<strong>MS</strong> Users Forum, simply go to www.agilent.com/chem/icpms<br />
and click on the <strong>ICP</strong>-<strong>MS</strong> User Forum link. First time visitors will need to<br />
register on the <strong>Agilent</strong> web site. New subscribers will also be prompted to<br />
enter their instrument serial number on their first visit only. Existing<br />
members will simply need to log in, as usual. Then simply click through<br />
to join the Forum.<br />
Please feel free to share your opinions on the <strong>ICP</strong>-<strong>MS</strong> User Forum with<br />
us at any time by sending an e-mail to karen@agilenticpms.com.<br />
Recent <strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> Publications<br />
To view and download these latest publications, go to<br />
www.agilent.com/chem/icpms and look under "Key Information"<br />
Technical Overview: ChemStation Software Suite for <strong>Agilent</strong> <strong>Technologies</strong> 7500 Series<br />
<strong>ICP</strong>-<strong>MS</strong>, 5989-0205EN<br />
Application Note: Fast and Accurate Determination of Arsenobetaine (AsB) in Fish<br />
Tissues using HPLC-<strong>ICP</strong>-<strong>MS</strong>, 5988-9893EN<br />
Application Note: Determination of Mercury in Microwave Digests of Foodstuffs by<br />
<strong>ICP</strong>-<strong>MS</strong>, 5989-0027EN<br />
Application Note: Speciation of Volatile Selenium Species in Plants using GC-<strong>ICP</strong>-<strong>MS</strong>,<br />
5988-9461EN<br />
<strong>Agilent</strong> <strong>ICP</strong>-<strong>MS</strong> <strong>Journal</strong> Editor<br />
Karen Morton for <strong>Agilent</strong> <strong>Technologies</strong><br />
e-mail: editor@agilent.com