Chromatography Forum

Hai

Any one having idea of simultaneously analysis of mesityl oxide and Diacetone alcohol by GC or HSGC. I need both LOQ below 10 ppm.

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what is the matrix?

Less than 10 ppm in WHAT ?

best wishes,

Rodney George

what is the matrix?

Less than 10 ppm in WHAT ?

best wishes,

Rodney George

I want to develop method for content of Mesityl Oxide and Diacetone alcohol content in one the API. I want to develop a method which should give below 10 ppm Limit of Quantitation for both the solvent.

Thank you

hi

Well hmm those are not exactly traditional residual solvents, so you may look at doing all development yourself. However I found a process related article (link below with some extract), indicating that a BP-5 or similar column might work resolution wise.

Personally I would firts try a traditional split injection (higher concentrated standards first) rather than a headspace injection first due to your aim for low LOQ and the fact that your targets are high boiling polar compounds (~130-170 °C) that may degrade/react at elevated headspace oven temperatures.

http://dspace.library.iitb.ac.in/jspui/ ... 1/5229.pdf

2.1.3. Analysis
A gas chromatograph (GC-911; Mak Anlytica India Ltd.)
equipped with flame ionization detector (FID) was used to
analyze the reaction mixture of acetone, MO and DAA. The
analysis was carried out in a 30m long BP-5 column (SGE,
Australia) with an inner diameter of 0.55mm. Elution was
established by nitrogen as a carrier gas at a flow rate of
0.5 ml/min.

hi

Well hmm those are not exactly traditional residual solvents, so you may look at doing all development yourself. However I found a process related article (link below with some extract), indicating that a BP-5 or similar column might work resolution wise.

Personally I would firts try a traditional split injection (higher concentrated standards first) rather than a headspace injection first due to your aim for low LOQ and the fact that your targets are high boiling polar compounds (~130-170 °C) that may degrade/react at elevated headspace oven temperatures.

http://dspace.library.iitb.ac.in/jspui/ ... 1/5229.pdf

2.1.3. Analysis
A gas chromatograph (GC-911; Mak Anlytica India Ltd.)
equipped with flame ionization detector (FID) was used to
analyze the reaction mixture of acetone, MO and DAA. The
analysis was carried out in a 30m long BP-5 column (SGE,
Australia) with an inner diameter of 0.55mm. Elution was
established by nitrogen as a carrier gas at a flow rate of
0.5 ml/min.

Thank you

I doing trail on DB-WAX (30M*0.32mm*0.25µ) thank you for your information

I understand if you are not able to tell the API matrix in which you seek to determine MO and DAA at 10 ppm.

The reactivity of the two analytes is the primary concern. Since you cannot tell us the matrix, can you tell us the possible dissolution solvent you would have to use to dissolve the matrix?

MIBK (similar to MO) is easily done by Headspace Analysis at temperatures below 90°.