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Research article
Fotouh Mansour
Tanta University Faculty of Pharmacy
Corresponding Author
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Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg /mL (correlation coefficient= 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µ g/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.
Keywords
Alogliptin, Plasma, Salting-out, Microextraction, Sitagliptin
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Editorial decision: Minor revision
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Editor invited
On 02 Nov, 2020
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Editorial decision: Major revision
On 10 Oct, 2020
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Received 07 Oct, 2020
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Received 07 Oct, 2020
Review #1 received
Received 29 Sep, 2020
Reviewer #3 agreed
On 11 Sep, 2020
Reviewer #1 agreed
On 10 Sep, 2020
Reviewer #2 agreed
On 10 Sep, 2020
Reviewers invited
Invitations sent on 02 Sep, 2020
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Subject Areas
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See the published version of this preprint at BMC Chemistry.
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Learn more about In Review
Research article
Fotouh Mansour
Tanta University Faculty of Pharmacy
Corresponding Author
Badges
Prescreen
This manuscript passed our Prescreen assessment
Complete author information
Appropriate declaration statements
Potential risks to human health
Prescreen
Peer Review Timeline
CURRENT STATUS: Published
View the published article at BMC Chemistry.
Version 4
Posted 28 Dec, 2020
No community comments so far
Editorial decision: Accept
On 07 Dec, 2020
Editor assigned
On 04 Dec, 2020
Submission checks complete
On 04 Dec, 2020
Editor invited
On 04 Dec, 2020
No comments provided
Reviewers invited
Invitations sent on 27 Nov, 2020
Reviewer #1 agreed
On 27 Nov, 2020
Review #1 received
Received 27 Nov, 2020
Editor assigned
On 26 Nov, 2020
Submission checks complete
On 26 Nov, 2020
Editor invited
On 26 Nov, 2020
No comments provided
Review #2 received
Received 15 Nov, 2020
Editorial decision: Minor revision
On 15 Nov, 2020
Reviewer #2 agreed
On 14 Nov, 2020
Reviewer #1 agreed
On 04 Nov, 2020
Review #1 received
Received 04 Nov, 2020
Editor assigned
On 02 Nov, 2020
Reviewers invited
Invitations sent on 02 Nov, 2020
Submission checks complete
On 02 Nov, 2020
Editor invited
On 02 Nov, 2020
No comments provided
Editorial decision: Major revision
On 10 Oct, 2020
Review #2 received
Received 07 Oct, 2020
Review #3 received
Received 07 Oct, 2020
Review #1 received
Received 29 Sep, 2020
Reviewer #3 agreed
On 11 Sep, 2020
Reviewer #1 agreed
On 10 Sep, 2020
Reviewer #2 agreed
On 10 Sep, 2020
Reviewers invited
Invitations sent on 02 Sep, 2020
Editor assigned
On 29 Aug, 2020
Submission checks complete
On 28 Aug, 2020
Editor invited
On 28 Aug, 2020
First submitted
On 27 Aug, 2020
Metrics
Comments: 0
PDF Downloads: ...
HTML Views: ...
Subject Areas
Analytical Chemistry
License:
This work is licensed under a CC BY 4.0 License. Read Full License
View the published article at BMC Chemistry.
Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg /mL (correlation coefficient= 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µ g/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.
Figure 1
Figure 2
Figure 3
Figure 4
Figure 5
Figure 6
Figure 7
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