Quantitative analysis of amorphous content of lactose using CCD-Raman spectroscopy

Pentti Niemelä (Corresponding Author), Maarit Päällysaho, Päivi Harjunen, Mikko Koivisto, Vesa-Pekka Lehto, Janne Suhonen, Kristiina Järvinen

Research output: Contribution to journal › Article › Scientific › peer-review

22 Citations (Scopus)

Abstract

A Raman spectroscopy method was developed for the quantification of the amorphous content of lactose. Both physical mixtures and spray-dried samples were used and the results were compared with the IMC determinations. Sample inhomogeneities were averaged out by collecting multiple spectra from each sample, and the total measurement time remained below 10 min due to the high sensitivity of the CCD-Raman spectrometer used in the measurements. The obtained calibration error (SEC) for the physical mixtures was 1.3% (w/w) in the 0–100% amorphous content range and was reduced to 0.2% (w/w) in the 0–10% range of more practical interest. The crystallization heat values of the spray-dried samples showed a linear correlation with the Raman quantifications in the amorphous content range of 0–80%, but saturated over the 80% concentration. This finding suggests a reference value of ca. 60 J/g for the spray-dried samples, instead of the crystallization heat of amorphous lactose (ca. 50 J/g) valid in the IMC determinations of physical mixtures.
Original languageEnglish
Pages (from-to)907-911
JournalJournal of Pharmaceutical and Biomedical Analysis
Volume37
Issue number5
DOIs
Publication statusPublished - 2005
MoE publication typeA1 Journal article-refereed

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Raman Spectrum Analysis
Lactose
Crystallization
Charge coupled devices
Raman spectroscopy
Hot Temperature
Chemical analysis
Calibration
Reference Values
Time measurement
Spectrometers

Keywords

  • Raman spectroscopy
  • quantification
  • amorphous content
  • lactose

Cite this

Niemelä, P., Päällysaho, M., Harjunen, P., Koivisto, M., Lehto, V-P., Suhonen, J., & Järvinen, K. (2005). Quantitative analysis of amorphous content of lactose using CCD-Raman spectroscopy. Journal of Pharmaceutical and Biomedical Analysis, 37(5), 907-911. https://doi.org/10.1016/j.jpba.2004.09.027
Niemelä, Pentti ; Päällysaho, Maarit ; Harjunen, Päivi ; Koivisto, Mikko ; Lehto, Vesa-Pekka ; Suhonen, Janne ; Järvinen, Kristiina. / Quantitative analysis of amorphous content of lactose using CCD-Raman spectroscopy. In: Journal of Pharmaceutical and Biomedical Analysis. 2005 ; Vol. 37, No. 5. pp. 907-911.
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Niemelä, P, Päällysaho, M, Harjunen, P, Koivisto, M, Lehto, V-P, Suhonen, J & Järvinen, K 2005, 'Quantitative analysis of amorphous content of lactose using CCD-Raman spectroscopy', Journal of Pharmaceutical and Biomedical Analysis, vol. 37, no. 5, pp. 907-911. https://doi.org/10.1016/j.jpba.2004.09.027

Quantitative analysis of amorphous content of lactose using CCD-Raman spectroscopy. / Niemelä, Pentti (Corresponding Author); Päällysaho, Maarit; Harjunen, Päivi; Koivisto, Mikko; Lehto, Vesa-Pekka; Suhonen, Janne; Järvinen, Kristiina.

In: Journal of Pharmaceutical and Biomedical Analysis, Vol. 37, No. 5, 2005, p. 907-911.

Research output: Contribution to journal › Article › Scientific › peer-review

TY - JOUR

T1 - Quantitative analysis of amorphous content of lactose using CCD-Raman spectroscopy

AU - Niemelä, Pentti

AU - Päällysaho, Maarit

AU - Harjunen, Päivi

AU - Koivisto, Mikko

AU - Lehto, Vesa-Pekka

AU - Suhonen, Janne

AU - Järvinen, Kristiina

PY - 2005

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N2 - A Raman spectroscopy method was developed for the quantification of the amorphous content of lactose. Both physical mixtures and spray-dried samples were used and the results were compared with the IMC determinations. Sample inhomogeneities were averaged out by collecting multiple spectra from each sample, and the total measurement time remained below 10 min due to the high sensitivity of the CCD-Raman spectrometer used in the measurements. The obtained calibration error (SEC) for the physical mixtures was 1.3% (w/w) in the 0–100% amorphous content range and was reduced to 0.2% (w/w) in the 0–10% range of more practical interest. The crystallization heat values of the spray-dried samples showed a linear correlation with the Raman quantifications in the amorphous content range of 0–80%, but saturated over the 80% concentration. This finding suggests a reference value of ca. 60 J/g for the spray-dried samples, instead of the crystallization heat of amorphous lactose (ca. 50 J/g) valid in the IMC determinations of physical mixtures.

AB - A Raman spectroscopy method was developed for the quantification of the amorphous content of lactose. Both physical mixtures and spray-dried samples were used and the results were compared with the IMC determinations. Sample inhomogeneities were averaged out by collecting multiple spectra from each sample, and the total measurement time remained below 10 min due to the high sensitivity of the CCD-Raman spectrometer used in the measurements. The obtained calibration error (SEC) for the physical mixtures was 1.3% (w/w) in the 0–100% amorphous content range and was reduced to 0.2% (w/w) in the 0–10% range of more practical interest. The crystallization heat values of the spray-dried samples showed a linear correlation with the Raman quantifications in the amorphous content range of 0–80%, but saturated over the 80% concentration. This finding suggests a reference value of ca. 60 J/g for the spray-dried samples, instead of the crystallization heat of amorphous lactose (ca. 50 J/g) valid in the IMC determinations of physical mixtures.

KW - Raman spectroscopy

KW - quantification

KW - amorphous content

KW - lactose

U2 - 10.1016/j.jpba.2004.09.027

DO - 10.1016/j.jpba.2004.09.027

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JO - Journal of Pharmaceutical and Biomedical Analysis

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Niemelä P, Päällysaho M, Harjunen P, Koivisto M, Lehto V-P, Suhonen J et al. Quantitative analysis of amorphous content of lactose using CCD-Raman spectroscopy. Journal of Pharmaceutical and Biomedical Analysis. 2005;37(5):907-911. https://doi.org/10.1016/j.jpba.2004.09.027

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