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NI NIR R ba base sed d ap approach proach to to eva evalu luate ate an anhy hydrate drate-hydra hydrate te tr tran ansformat sformations ions Dha hara a Ra Raij ijada, a, Ki Kinja jal l Koradia ia, Mia , Mia La Lars

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SLIDE 1

NI NIR R ba base sed d ap approach proach to to eva evalu luate ate an anhy hydrate drate-hydra hydrate te tr tran ansformat sformations ions

Dha hara a Ra Raij ijada, a, Ki Kinja jal l Koradia ia, Mia , Mia La Lars rsen, , Vis isha hal l Koradia ia, , Cla laus us Corn rnett, tt, Juk ukka ka Ra Rantan anen

Elect ectronic

  • nic Co

Conferen erence ce on Ph Pharmaceutical maceutical Sc Sciences ences ECP CPS2 S2011/F 011/Futu ture re Mnauf ufact cturing uring of Ph Pharmaceu maceutical icals

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ECPS 2011/Future Manufacturing of Pharmaceuticals

In Intro roducti duction

  • n
  • Need for PAT tools in pharmaceutical development
  • NIR spectroscopy as a PAT tool

So Solid lid fo form rms of s of Na Napr prox

  • xen

en so sodi dium um (N (NS) S) Ob Object jective ive of

  • f th

the pr e pres esen ent t wo work rk Re Resu sult lts

  • TGA and PXRD patterns
  • FTIR and NIR spectra
  • Scores and loadings plot from NIR spectra

Su Summ mmary ary

2

Ou Outline tline

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ECPS 2011/Future Manufacturing of Pharmaceuticals 3

Need eed fo for Pr r Proc

  • cess

ess An Analy alytical tical Te Techn chnol

  • log
  • gy

y to tool

  • ls

“QUALITY PHARMACEUTICAL PRODUCT”

Understanding of the solid form during various phases of development : Crucial factor

Important to identify suitable technique during early development that can monitor such changes and can be developed as a PAT tool for future manufacturing of pharmaceutical products

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SLIDE 4

ECPS 2011/Future Manufacturing of Pharmaceuticals

Fast, noninvasive and real time data acquisition possibilities makes NIR as

  • ne of the ideal PAT tools

Multivariate data analysis from NIR spectral data can provide simple and quick approach for extracting information from NIR spectral data

4

NIR IR Sp Specro ecrosco scopy py as a as a PA PAT to T tool

  • l

Katherine A. Bakeev, Pharmaceutical Technology Europe, Sep. 2003

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ECPS 2011/Future Manufacturing of Pharmaceuticals 5

So Solid lid fo form rms s of

  • f Na

Napro proxen xen So Sodium dium

AH: Anhydrate, MH: Monohydrate, DH: Dihydrate, TH: Tetrahydrate

AH MH TH DH

Methanol-water mixture (64mol% methanol)

60° C 53% RH 94% RH 20 days

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SLIDE 6

ECPS 2011/Future Manufacturing of Pharmaceuticals 6

Ob Objective jective of

  • f t

the pr he present esent wor

  • rk

1Bansal, P. et. al. Drug Dev. Ind. Pharm. 1994, 20, 2151-2156; 2Martino, P.D.et.al, J. Pharm. Sci. 2008, 97, 5263-5273.

Alteration in physicochemical properties of NS, attributed to the anhydrate to hydrate transformation during processing, has been reported1,2 However, till date no PAT tool has been evaluated for monitoring of phase transformation of NS during pharmaceutical processing..!! Therefore, the present study focuses on evaluating feasibility of NIR spectroscopy as a real-time monitoring tool

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ECPS 2011/Future Manufacturing of Pharmaceuticals 7

Th Ther ermal mal Gr Grav avim imetri etric c An Anal alysis ysis

6.59% 12.03% 21.67%

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ECPS 2011/Future Manufacturing of Pharmaceuticals 8

PX PXRD RD pa patt tterns erns

Note:The dotted diffractograms are the calculated patterns for AH and MH forms from their crystal structures

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SLIDE 9

ECPS 2011/Future Manufacturing of Pharmaceuticals 9

1229

FTI TIR R spe spect ctra ra

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ECPS 2011/Future Manufacturing of Pharmaceuticals 10

NIR Spe IR Spect ctra ra (S (SNV V co corr rrect ected) ed)

O-H 1st Overtone O-H combination C-H 1st Overtone C-H combination

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ECPS 2011/Future Manufacturing of Pharmaceuticals 11

Ch Chemical emical in info forma rmation ion fr from

  • m FT

FTIR a IR and d NI NIR R sp spec ectra ra

Soli lid for

  • rm

O-H H stre retching tching (F (FTI TIR) R) 1st

st O-H

H Ov Overt rton

  • ne (t

(theo eoretical retical*) *) 1st

st O-H

H Ov Overt rton

  • ne

(e (expe peri rimen ental#) MH 3450 cm-1 6900 cm-1 (1449 nm) 1446 nm DH 3350 cm-1 6700 cm-1 (1492 nm) 1496 nm TH 3450-3380 cm-1 6900-6760 cm-1 (1449-1479 nm) 1447-1465 nm

1229

*calculated by multiplying the wave-number values for fundamental vibrations in FTIR spectra by 2; #observed by NIR spectroscopy

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ECPS 2011/Future Manufacturing of Pharmaceuticals 12

  • 30
  • 20
  • 10

10 20 30

  • 15
  • 10
  • 5

5 10 15 Scores on PC 1 (81.62%) Scores on PC 2 (13.63%)

TH DH MH AH

TH (Selected) 95% Confidence Level

PC PCA A Sco Score res s plo lot fro t from m NIR spe IR spect ctral ral da data ta

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SLIDE 13

1200 1400 1600 1800 2000 2200

  • 0.08
  • 0.06
  • 0.04
  • 0.02

0.02 0.04 0.06 0.08 Variable Loadings on PC 1 (81.62%) 1200 1400 1600 1800 2000 2200

  • 0.06
  • 0.04
  • 0.02

0.02 0.04 0.06 0.08 0.1 Variable Loadings on PC 2 (13.63%)

ECPS 2011/Future Manufacturing of Pharmaceuticals

PC PCA A Lo Load ading ings s pl plot fro t from m NIR spe IR spect ctral ral da data ta

13

Loadings on PC1 Loadings on PC2

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ECPS 2011/Future Manufacturing of Pharmaceuticals 14

Co Conclusion nclusion

 NIR spectroscopy coupled with multivariate data analysis can efficiently distinguish the NS solid forms  NIR spectroscopy can be considered as a potential technique to monitor phase transformations  Further studies will focus on development of NIR based quantitative model that can be applied for real time monitoring

  • f

hydrate formation and dehydration behaviour of the NS solid forms during processing and storage

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ECPS 2011/Future Manufacturing of Pharmaceuticals 15