Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy

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Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy. / Warnecke, Solveig; Wu, Jian X.; Rinnan, Åsmund; Allesø, Morten; van den Berg, Frans; Jepsen, Peter Uhd; Engelsen, Søren Balling.

In: Vibrational Spectroscopy, Vol. 102, 2019, p. 39-46.

Research output: Contribution to journalJournal articleResearchpeer-review

Harvard

Warnecke, S, Wu, JX, Rinnan, Å, Allesø, M, van den Berg, F, Jepsen, PU & Engelsen, SB 2019, 'Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy', Vibrational Spectroscopy, vol. 102, pp. 39-46. https://doi.org/10.1016/j.vibspec.2019.03.004

APA

Warnecke, S., Wu, J. X., Rinnan, Å., Allesø, M., van den Berg, F., Jepsen, P. U., & Engelsen, S. B. (2019). Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy. Vibrational Spectroscopy, 102, 39-46. https://doi.org/10.1016/j.vibspec.2019.03.004

Vancouver

Warnecke S, Wu JX, Rinnan Å, Allesø M, van den Berg F, Jepsen PU et al. Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy. Vibrational Spectroscopy. 2019;102:39-46. https://doi.org/10.1016/j.vibspec.2019.03.004

Author

Warnecke, Solveig ; Wu, Jian X. ; Rinnan, Åsmund ; Allesø, Morten ; van den Berg, Frans ; Jepsen, Peter Uhd ; Engelsen, Søren Balling. / Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy. In: Vibrational Spectroscopy. 2019 ; Vol. 102. pp. 39-46.

Bibtex

@article{14610d60ff3247c08a74c95c9b75aa5d,
title = "Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy",
abstract = "Spray-dried lactose consists of an amorphous component (10–20{\%}) as well as the crystalline monohydrate form [1]. It is commonly used as a diluent in direct compression, mainly because of its better flow characteristics compared to pure crystalline lactose. The amorphous form is metastable and can relative easily crystallize, which will affect the functionality of the pharmaceutical product. It is therefore of interest to establish methods for non-invasive and rapid assessment of the level of crystallinity in a pharmaceutical formulation. In this study, two spectroscopic methods, near infrared (NIR) spectroscopy and terahertz time domain spectroscopy (THz-TDS), are compared for their ability to determine low levels of crystalline lactose in a mixture. The aim was to find the limit of detection and limit of quantification for the two techniques. Partial least squares (PLS) regression models were developed and the root-mean-square-error-of-cross-validation (RMSECV) for the models with full concentration range were found to be 2.91{\%} (w/w) and 0.87{\%} (w/w) for THz-TDS and NIR, respectively. Calibrations developed on samples containing 0–10{\%} (w/w) crystalline material resulted in RMSECVs of 0.30{\%} (w/w) and 0.20{\%} (w/w) for THz-TDS and NIR, respectively, while the limits of detection were 0.80{\%} (w/w) and 0.43{\%} (w/w), respectively. Both instrumental techniques are thus able to quantify the content of crystalline lactose in a mixture. To select one method over the other in an industrial quality assurance setting, further includes other aspects - such as sample handling, sample size, outlier information, instrument stability, etc. In all these aspects, NIR spectroscopy currently performs better than THz-TDS.",
keywords = "Amorphous, Crystalline, Lactose, Limit of detection (LOD), NIR, Terahertz time domain spectroscopy (THz-TDS)",
author = "Solveig Warnecke and Wu, {Jian X.} and {\AA}smund Rinnan and Morten Alles{\o} and {van den Berg}, Frans and Jepsen, {Peter Uhd} and Engelsen, {S{\o}ren Balling}",
year = "2019",
doi = "10.1016/j.vibspec.2019.03.004",
language = "English",
volume = "102",
pages = "39--46",
journal = "Analytica Chimica Acta",
issn = "0003-2670",
publisher = "Elsevier",

}

RIS

TY - JOUR

T1 - Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy

AU - Warnecke, Solveig

AU - Wu, Jian X.

AU - Rinnan, Åsmund

AU - Allesø, Morten

AU - van den Berg, Frans

AU - Jepsen, Peter Uhd

AU - Engelsen, Søren Balling

PY - 2019

Y1 - 2019

N2 - Spray-dried lactose consists of an amorphous component (10–20%) as well as the crystalline monohydrate form [1]. It is commonly used as a diluent in direct compression, mainly because of its better flow characteristics compared to pure crystalline lactose. The amorphous form is metastable and can relative easily crystallize, which will affect the functionality of the pharmaceutical product. It is therefore of interest to establish methods for non-invasive and rapid assessment of the level of crystallinity in a pharmaceutical formulation. In this study, two spectroscopic methods, near infrared (NIR) spectroscopy and terahertz time domain spectroscopy (THz-TDS), are compared for their ability to determine low levels of crystalline lactose in a mixture. The aim was to find the limit of detection and limit of quantification for the two techniques. Partial least squares (PLS) regression models were developed and the root-mean-square-error-of-cross-validation (RMSECV) for the models with full concentration range were found to be 2.91% (w/w) and 0.87% (w/w) for THz-TDS and NIR, respectively. Calibrations developed on samples containing 0–10% (w/w) crystalline material resulted in RMSECVs of 0.30% (w/w) and 0.20% (w/w) for THz-TDS and NIR, respectively, while the limits of detection were 0.80% (w/w) and 0.43% (w/w), respectively. Both instrumental techniques are thus able to quantify the content of crystalline lactose in a mixture. To select one method over the other in an industrial quality assurance setting, further includes other aspects - such as sample handling, sample size, outlier information, instrument stability, etc. In all these aspects, NIR spectroscopy currently performs better than THz-TDS.

AB - Spray-dried lactose consists of an amorphous component (10–20%) as well as the crystalline monohydrate form [1]. It is commonly used as a diluent in direct compression, mainly because of its better flow characteristics compared to pure crystalline lactose. The amorphous form is metastable and can relative easily crystallize, which will affect the functionality of the pharmaceutical product. It is therefore of interest to establish methods for non-invasive and rapid assessment of the level of crystallinity in a pharmaceutical formulation. In this study, two spectroscopic methods, near infrared (NIR) spectroscopy and terahertz time domain spectroscopy (THz-TDS), are compared for their ability to determine low levels of crystalline lactose in a mixture. The aim was to find the limit of detection and limit of quantification for the two techniques. Partial least squares (PLS) regression models were developed and the root-mean-square-error-of-cross-validation (RMSECV) for the models with full concentration range were found to be 2.91% (w/w) and 0.87% (w/w) for THz-TDS and NIR, respectively. Calibrations developed on samples containing 0–10% (w/w) crystalline material resulted in RMSECVs of 0.30% (w/w) and 0.20% (w/w) for THz-TDS and NIR, respectively, while the limits of detection were 0.80% (w/w) and 0.43% (w/w), respectively. Both instrumental techniques are thus able to quantify the content of crystalline lactose in a mixture. To select one method over the other in an industrial quality assurance setting, further includes other aspects - such as sample handling, sample size, outlier information, instrument stability, etc. In all these aspects, NIR spectroscopy currently performs better than THz-TDS.

KW - Amorphous

KW - Crystalline

KW - Lactose

KW - Limit of detection (LOD)

KW - NIR

KW - Terahertz time domain spectroscopy (THz-TDS)

U2 - 10.1016/j.vibspec.2019.03.004

DO - 10.1016/j.vibspec.2019.03.004

M3 - Journal article

AN - SCOPUS:85064152147

VL - 102

SP - 39

EP - 46

JO - Analytica Chimica Acta

JF - Analytica Chimica Acta

SN - 0003-2670

ER -

ID: 217996084