Elemental and Heavy Metal Screening

Quantitative Heavy Metal Screening by ICP-OES



When to Choose

This method covers impurities of the most common heavy
metals in organic compounds.
This quantitative and GMP-compliant method yields data
that can be readily used in registration dossiers.
Depending on the matrix, this method has better LOQs for
Fe, V, and Al than ICP-MS.


Determined Elements
Package 1: 18 elements (Al, As, Ba, Cd, Co, Cr, Cu, Fe, Mn, Mo,
Ni, Pb, Pd, Se, Sn, Ti, V, Zn)
Package 2: 21 elements (all Package 1 elements plus Bi, Pt, Sb)


Method

ICP-OES after a wet decomposition step
The method corresponds Ph. Eur. 2.2.57. (inductively coupled plasma-atomic emission spectrometry) and to USP method
<730> Plasma Spectrochemistry.


Limit of Quantitation

Typically 1 mg/kg for each element


Suitable Matrix

Organic compounds


Sample Amount

200 mg (single determination) or 400 mg (duplicate determination)


Available under GMP

Yes



Quantitative Determination of USP Heavy Metals by ICP-MS

When to choose

This method can be used as an alternative to the USP <231>
heavy metal test and the related Ph. Eur. 2.4.8 test, particularly when
quantitative and reliable values are required for each individual metal.


Determined Elements

Ag, As, Bi, Cd, Cu, Hg, Mo, Pb, Sb, Sn (mentioned in USP <231> Heavy Metals

as those elements that typically respond)

Method

ICP-MS after a wet decomposition step

The method complies with USP <730> Plasma Spectrochemistry.


Limit of Quantitation

Between 0.1 and 0.5 mg/kg for each element


Suitable Matrix

Organic compounds


Sample amount

200 mg (single determination) or 400 mg (duplicate determination)


Available under GMP

Yes


Semi-Quantitative Metal Screening by ICP-MS

When to choose
This method provides a general overview of metal and semi-metal traces in
organic samples covering the entire periodic table
For many elements this method has a better LOQ than ICP-OES.


Determined elements

All metals and semi-metals from lithium to uranium

Method
ICP-MS after a wet decomposition test.

Limit of quantitation
Between 0.1 and 1 mg/kg for each element, excluding Al, Ca, Fe and K
(LOQs between 1 and 10 mg/kg)

Suitable matrix
Organic compounds

Sample amount
200 mg (single determination)

Available under GMP
No



Semi-Quantitative Element Screening by XRF


When to Choose

This method provides a general overview of the elemental composition and
impurities of a sample.
Not limited to organic compounds.

Determined Elements
All elements from sodium to uranium, including Si, P, S, Cl, Br, and I.
Elements are classified into 4 categories:
• Major elements contributing >5% by weight
• Minor elements contributing 1–5% by weight
• Minor elements contributing >0.1–1% by weight
• Trace elements contributing <0.1% by weight
Identified elements can be quantified using WDXRF or other methods
upon request.

Method
Direct analysis by energy and wavelength dispersive X-ray fluorescence
spectrometry
The WDXRF method corresponds to the Ph. Eur. method 2.2.37 X-ray
Fluorescence Spectrometry

Limit of Quantitation
Between 1 and 50 mg/kg for each element, depending on element, amount
of substance and matrix

Suitable Matrix
Any kind of liquid and solid test material, even unknown materials such as
residues and abrasions

Sample Amount
0.1 to 4 g; best semi-quantitative classification is obtained with ≥ 3 g

Available under GMP
No