Determination of EDTA Content in ppm or ppb levels

Chromatography Forum: LC Archives: Determination of EDTA Content in ppm or ppb levels
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Saturday, September 21, 2002 - 12:55 am:

can any one tell about Determination of EDTA Content in ppm or ppb levels in one of the Active pharmaceutical Ingrediants preferably
hplc or any other method.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By maris on Saturday, September 21, 2002 - 09:25 am:

Probably I can give you some recommendations.
Please mail me directly.

Dr.Alex Weisman


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Chris Pohl on Monday, September 23, 2002 - 09:31 am:

There are a number of options for the analysis of EDTA. One method involves separation of EDTA at low pH via cation exchange with post-column derivitization using an iron based detection system. This method is detailed in: Ion Chromatography, second edition, page 133, by Joachim Weiss, published by VCH. It is also possible to separate EDTA as a metal complex with UV detection. Although I don't have the specifics, I know I've seen methods involving detection of EDTA as a copper complex at pH 5-6 via anion exchange. It can also be separated directly via anion exchange but in this case it is crucial that no metals be present (i.e. a chelating trap column must be placed before the injection valve and column hardware should be nonmetallic). Even with these precautions it can be challenging to quantitate EDTA directly because the sample itself may contain various amounts of metal which will result in multiple peaks.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Monday, September 23, 2002 - 03:31 pm:

I use an application for NTA, EDTA and DTPA using a Protosil 120-5 ODSAQ (reversed phase)column in waste waters
The samples are reacted with Fe3+
The eluent is 0.5mmol/L HNO3, 2.5 mmol/L Tetra Butyl Ammoonium Hydroxide, 7.5 mmol/L Tetra ammonium hydrogen sulphate,, 5% Methanol, at 1.0ml/min
The suppressor in use is the Metrohm Suppressor Module (MSM) which can be used with Metrohm and non-metrohm HPLC kit.
The use of the Metrohm MSM reduces matrix interferrence, esp. the large injection peak from the Fe3+ in the sample and therefore allows lower detection limits for EDTA + NTA
Good peak height for 10ug/L (ppb)for EDTA
Look at site for details
://www.metrohm.com/docs/app/notes/pdf/s36.pdf
for a pdf file download.
I use the method. It is robust.
It works very well.
good luck


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Monday, September 23, 2002 - 03:32 pm:

I use an application for NTA, EDTA and DTPA using a Protosil 120-5 ODSAQ (reversed phase)column in waste waters
The samples are reacted with Fe3+
The eluent is 0.5mmol/L HNO3, 2.5 mmol/L Tetra Butyl Ammoonium Hydroxide, 7.5 mmol/L Tetra ammonium hydrogen sulphate,, 5% Methanol, at 1.0ml/min
The suppressor in use is the Metrohm Suppressor Module (MSM) which can be used with Metrohm and non-metrohm HPLC kit.
The use of the Metrohm MSM reduces matrix interferrence, esp. the large injection peak from the Fe3+ in the sample and therefore allows lower detection limits for EDTA + NTA
Good peak height for 10ug/L (ppb)for EDTA
Look at site for details
://www.metrohm.com/docs/app/notes/pdf/s36.pdf
for a pdf file download.
I use the method. It is robust.
It works very well.
good luck
Probably make sure system is in PEEK through out


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Tuesday, September 24, 2002 - 06:31 am:

Surely you would only need PEEK from just the suppressor to detector ????


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Chris Pohl on Tuesday, September 24, 2002 - 09:35 am:

Anon (Tuesday Sept. 24),

Actually, it is not sufficient to simply use PEEK between the suppressor and the detector (I know this from actual experience). If you are attempting to separate the EDTA as the uncomplexed anion at pH > 5, you must prevent the analyte from coming in contact with any metal. Otherwise, you will observe multiple peaks or severe peak asymmetry depending upon the analytical system. The largest source of metals actually turns out to be electrolytes present in the mobile phase but other possible major sources are the eluent bottle filter (if it's composed of metal), the inlet and outlet frit in the column (if they are metallic frits). Connecting tubing and the column body can also be a problem if they are of metallic composition although they represent a much less significant contamination sources considering their relatively low surface area of exposed metal.


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