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Studying Systematic Errors on Estimation Decision, Detection, and Quantification Limit on Micro-TLC

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Abstract

The decision limit (CCα), capability of detection (CCβ) and quantification limit (QL) are importance performance characteristics in method validation. The TLC-Scanner 3 from Camag provides the possibility to choose the slit dimension of light to determine the peak chromatogram of a substance. The influence of the slit dimension for determination of CCα, CCβ and QL of paracetamol has been carried out. Paracetamol was spotted onto plates of AL-TLC Si G 60 F254 by linomat 4 in the range of 50–400 ng/spot and 10–400 ng/band, then on twin chambers eluted with TAEA (toluene:acetone-ethanol:conc.ammonia, 45 + 45 + 7 + 3 v/v) for 45 mm. Eluted spots were scanned in different slit dimensions at 248 nm. The CCα, CCβ and QL of paracetamol were estimated through the linear regression (LRM) and signal-to-noise (S/N) methods. Slit lengths between 50 and 133 % of the band width of the spots, and with the noise factor of the slit under 2.6, produced good precision measurements of TLC-densitometry between plates, while slit lengths between 50 and 83 % of the band width of the spots introduced a higher sensitivity response of the detector. The estimated CCα, CCβ and QL were determined by how the data were collected, the analytical optical setting, and the usage method for the estimation of both validation parameters.

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Authors and Affiliations

  1. Pharmacy Department, Faculty of Mathematic and Natural Science, Udayana University, Denpasar, Indonesia

    I Made Agus Gelgel Wirasuta, Ni Made Amelia Ratnata Dewi, Kadek Duwi Cahyadi, Luh Putu Mirah Kusuma Dewi, Ni Made Widi Astuti & I Nyoman Kadjeng Widjaja

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  1. I Made Agus Gelgel Wirasuta
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  2. Ni Made Amelia Ratnata Dewi
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  3. Kadek Duwi Cahyadi
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  4. Luh Putu Mirah Kusuma Dewi
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  5. Ni Made Widi Astuti
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  6. I Nyoman Kadjeng Widjaja
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Correspondence to I Made Agus Gelgel Wirasuta.

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Published in the topical collection Miniaturized and New Featured Planar Chromatography and Related Techniques with guest editor Paweł K. Zarzycki.

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Wirasuta, I.M.A.G., Dewi, N.M.A.R., Cahyadi, K.D. et al. Studying Systematic Errors on Estimation Decision, Detection, and Quantification Limit on Micro-TLC. Chromatographia 76, 1261–1269 (2013). https://doi.org/10.1007/s10337-012-2376-4

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  • DOI: https://doi.org/10.1007/s10337-012-2376-4

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