As per USP 38 column temperature mentioned as Column temperature: Beginning of column, 50°; end of column, 35° for Lumenfantrine by HPLC This created lots of confusion could anyone clarify on this whether this is column oven temperature programming in method or kept different temperature on both end of column which is not feasible.
As per
http://www.usp.org/sites/default/files/usp_pdf/EN/compendial_deferrals_for_usp37.pdf.pdf
"Monograph/Section(s): Lumefantrine/Assay
Expert Committee(s): Monographs—Small Molecules 1
No. of Commenters: 1
Comment Summary #1: The commenter requested replacing the temperature gradient across the column with a constant column temperature of 40o.
Response: Comment not incorporated. The Expert Committee will consider further revisions to the monograph upon the receipt of the necessary supporting data. "
Apparently the USP 38 monograph specifies a temperature gradient over the column, I suggest holding the column temperature at 40C as the commenter suggests.
Thanks a lot Mr. Bruce Levison, Could please share any other supporting document which specifies analysis of Lumefantrine/Assay by holding column temperature at 40C in stead of setting different temperatures at both ends of column.
A search of the articles on this topic from Scifinder failed to provide any supporting documentation for analysis of Lumefantrine by holding the column temperature at 40C most analyses specify 30C. I suggest contacting the USP directly at: [email protected]
Dear Mr. Bruce Levison,
Thanks for your suggestion, i had contacted USP and they responded (response given below)
This method is instrument specific. The sponsor validated the method using those oven conditions-different temperature at each end of the column. For your information, the sponsor used a Agilent 1200 Fast HPLC which is capable of establishing the temperature difference cited in the monograph. The USP lab also used an Agilent system when conducting this method.
Using different conditions may be considered an alternative method and would need to be validated as per USP General Notices (section 6.30):
"6.30. Alternative and Harmonized Methods and Procedures
Alternative methods and/or procedures may be used if they provide advantages in terms of accuracy, sensitivity, precision, selectivity, or adaptability to automation or computerized data reduction, or in other special circumstances. Such alternative procedures and methods shall be validated as described in the general chapter Validation of Compendial Procedures and must be shown to give equivalent or better results. Only those results obtained by the methods and procedures given in the compendium are conclusive.
Alternative procedures should be submitted to USP for evaluation as a potential replacement or addition to the standard (see section 4.10, Monographs).
Certain general chapters contain a statement that the text in question is harmonized with the corresponding text of the European Pharmacopoeia and/or the Japanese Pharmacopoeia and that these texts are interchangeable. Therefore, if a substance or preparation is found to comply with a requirement using an interchangeable method or procedure from one of these pharmacopeias, it should comply with the requirements of the USP. When a difference appears, or in the event of dispute, only the result obtained by the method and/or procedure given in the USP is conclusive.”
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