ICPMS PRESENTATION

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An analytical technique to
determine Elements using
Mass Spectrometry from
Ions generated by an
Inductively
Coupled Plasma

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Liquid droplets are formed on the tip of
a needle, where
they become nebulized due to argon
gas flowing through a second needle
perpendicular to the
sample needle.

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Aerosol passes into
spray chamber where
large droplets are
removed via a drain.
Only 2% of original mist
enters the spray
chamber.

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Ion optics – guides the
desired ions into the
quadrupole
while assuring that
neutral species are
discarded from the ion
beam

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Quadrupole works as a mass
filter
Separates ions based on
mass/charge ratio
Analyzes more than 40
elements in less than 1 second!

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ions hit the surface of the detector
and are converted to electrons
counts individual ions exiting the
quadrupole.

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Wide Elemental Coverage
Almost every element can be
measured
Very low detection limits
Equivalent to or lower than GFAAS
(single-element technique) and
ICP OES
Multi-element analysis in 3 to 4
minutes
Relatively few interferences

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AAS: Single element, ppm/ppb range
Cheap, simple
Small dynamic range
GFAAS about 100 times more sensitive than FAAS, but
also more challenging
ICP-OES: Multi-element, ppb range
Limited spectral interferences, good stability, low matrix
effects
ICP-MS: Multi-element, possible to reach ppt
Most complex, most expensive, lowest detection limits,
isotope analysis possible

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The term heavy metal
refers to any metallic
chemical element that
has a relatively high
density and is toxic or
poisonous at low
concentrations.

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The current USP method used for
monitoring
inorganic contaminants in
pharmaceutical samples
is a 100 year-old colorimetric
test, defined in General
Chapter <231>.

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Heavy metals limit test is based on
precipitation of 10
sulfide-forming elements (Ag, As, Bi, Cd, Cu,
Hg, Mo,Pb, Sb and Sn), in a reaction with a
reagent such as
thioacetamide. The resulting colored
precipitate is
compared visually to a 10 ppm Pb standard
to determine
compliance with the heavy metal limit

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USP<231> is a limit test based
on the sum of the 10 elements, and so
does not give
individual concentrations for each
element. Also, it
cannot be used for the determination of
many elements
of interest such as Cr, and the platinum
group elements
that are commonly used as production
catalysts.

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Class 1: (As, Cd, Hg and Pb): Highly toxic
across all administration routes. These
require special consideration during the
risk assessment, due to their high toxicity
and the potential for them to be present in
finished dosage
Class 2: (V, Mo, Se, and Co )
(Au, Tl, Pd, Pt, Ir, Os, Rh, Ag and Ru)
Toxic to a greater or lesser extent based on
route
of administration.

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Class 3:
Sb, Ba, Li, Cr, Cu, Sn, and Ni.
Relatively low toxicity by oral route of
administration, but require consideration in
the risk assessment for other routes of
administration.
Class 4:
Al, B, Fe, Zn, K, Ca, Na, Mn, Mg, and W.
Elemental impurities that have been
evaluated
but for which a PDE has not been established
due to their low inherent toxicity and/or
regional regulations.

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Element Class Oral Inhalation PDE, μg/day
As 1 15 1.9
Cd 1 5.0 3.4
Hg 1 40 1.2
Pb 1 5.0 5.0

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