15.11.2012 Views

Preparation of a standard Melamine solution

Preparation of a standard Melamine solution

Preparation of a standard Melamine solution

SHOW MORE
SHOW LESS

Create successful ePaper yourself

Turn your PDF publications into a flip-book with our unique Google optimized e-Paper software.

Regarding the <strong>Melamine</strong> Crisis<br />

Methods for <strong>Melamine</strong> Analysis via HPLC<br />

There are basically 2 methods we can <strong>of</strong>fer via HPLC,<br />

depending on the requirements <strong>of</strong> the employed equipment:<br />

1 st Method: Reversed Phase Mode<br />

U.S. FDA states to use a commercially available C8 column for the analysis <strong>of</strong> <strong>Melamine</strong>.<br />

Very promising results can be obtained with Inertsil C8-3<br />

Inertsil C8-3 5um 4.6X150mm or 250mm<br />

(Cat# 5020-01900 or 5020-01901)<br />

Important Remarks on the 1 st method: Reversed Phase Mode<br />

An ion-pair reagent is used in this application.<br />

Therefore, this application is NOT compatible with LC/MS/MS analysis.<br />

This is due to the fact that an ion-pair reagent will heavily contaminate the expensive LC/MS detector.<br />

This application data is ONLY compatible with instrumental setups employing an UV or PDA detector.<br />

2 nd Method: For LC/MS/MS<br />

Please see Slide 3


Regarding the <strong>Melamine</strong> Crisis<br />

1st Method: Reversed Phase Mode, Inertsil C8-3 5um 4.6X150mm


Regarding the <strong>Melamine</strong> Crisis<br />

1st Method: Reversed Phase Mode, Inertsil C8-3 5um 4.6X250mm


Regarding the <strong>Melamine</strong> Crisis<br />

LC/MS/MS-Method<br />

2 nd Method: For LC/MS/MS<br />

If you will be using a LC/MS/MS, please use the following:<br />

Inertsil HILIC 5um 3.0X150mm on LC/MS/MS-System<br />

(Cat# 5020-07715)<br />

Important Remarks on the 2 nd method: For LC/MS/MS<br />

The mobile phase used in this application data is compatible with LC/MS/MS.


4<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


5<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


6<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


7<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


8<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


9<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


10<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


11<br />

Regarding the <strong>Melamine</strong> Crisis<br />

2 nd Method: For LC/MS/MS, Inertsil HILIC 5um 3.0X150mm


12<br />

Regarding the <strong>Melamine</strong> Crisis<br />

<strong>Preparation</strong> <strong>of</strong> a <strong>standard</strong> <strong>Melamine</strong> <strong>solution</strong><br />

Background information <strong>of</strong> <strong>Melamine</strong> (2, 4, 6-triamine-s-triazine)<br />

It is only slightly soluble in water.<br />

It is soluble to warm (hot) water and diluted hydrochloric acid.<br />

However, it is insoluble in hydrophobic solvents.<br />

<strong>Preparation</strong> <strong>of</strong> <strong>standard</strong> stock <strong>solution</strong> <strong>of</strong> <strong>Melamine</strong><br />

1) Measure 50mg <strong>of</strong> <strong>Melamine</strong>.<br />

2) Dissolve it by 20% Methanol <strong>solution</strong> and making it at 50mL.<br />

3) Use this <strong>solution</strong> as a 1,000ppm <strong>standard</strong> stock <strong>solution</strong>.<br />

<strong>Preparation</strong> <strong>of</strong> <strong>standard</strong> <strong>Melamine</strong> <strong>solution</strong><br />

1) Whenever using the above <strong>standard</strong> stock <strong>solution</strong>, always add 1% trichloroacetic acid and dilute it.<br />

2) Then use the <strong>solution</strong> as a <strong>standard</strong> <strong>Melamine</strong> <strong>solution</strong>.<br />

For example:<br />

1) Take 1mL <strong>of</strong> the <strong>standard</strong> stock <strong>solution</strong> and add 1% trichloroacetic acid and make it at 10mL.<br />

2) This 10mL will be the <strong>standard</strong> <strong>Melamine</strong> <strong>solution</strong>.<br />

3) In this case, 0.1mg <strong>of</strong> <strong>Melamine</strong> will be contained in a 1mL <strong>of</strong> <strong>standard</strong> <strong>Melamine</strong> <strong>solution</strong>.


13<br />

Regarding the <strong>Melamine</strong> Crisis<br />

Procedure <strong>of</strong> Sample <strong>Preparation</strong>


14<br />

Regarding the <strong>Melamine</strong> Crisis<br />

Solid Phase Extraction Method


15<br />

Regarding the <strong>Melamine</strong> Crisis<br />

Ordering Information<br />

* For price information, please send a quotation request:<br />

Info@mz-at.de?subject=melamin-analytics

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!