2011Qilu Pharmaceutical AffairsRequires access

Rapid nondestructive quantitative analysis of Nicotinamide Tablets by near infrared diffuse reflectance spectrometry

Bingren Xiang

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Abstract

Objective To develop a near infrared diffuse reflectance analysis(NIRDRA)method for rapid nondestructive quantitative determination of nicotinamide in tablets.Methods All spectra were measured by a Fourier transform spectrometer equipped with a PbS and a InGaAs detector,an external integrating sphere and a fibre-optic probe for reflectance measurements.All samples were scanned from 12 000 cm-1 to 4 000 cm-1,and each spectrum was obtained though automatic mean of 64 scans.First derivative spectrum preprocessing method was used,and spectral region(9 750.7~7 498.2 cm-1)was selected to develop mathematical models by partial least square method for nicotinamide tablets samples.Results The optimal rank and mean square error determined for samples though automatic mean of 64 scans by cross validation method were 4 and 3.34 respectively;the average recovery was 99.56%;and the RSD was 2.58%.To verify that the NIR method was feasible for application,the predicted values were compared to the observed values measured by HPLC which was used as the reference method.The paired t-test was applied and the results showed that there was no significant difference between the NIR method and the reference methods(P0.05).Conclusion The NIRDRA method was rapid,simple,and noninvasive,and it can be applied to assay for the content of nicotinamide in tablets.

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Objective To develop a near infrared diffuse reflectance analysis(NIRDRA)method for rapid nondestructive quantitative determination of nicotinamide in tablets.Methods All spectra were measured by a Fourier transform spectrometer equipped with a PbS and a InGaAs detector,an external integrating sphere and a fibre-optic probe for reflectance measurements.All samples were scanned from 12 000 cm-1 to 4 000 cm-1,and each spectrum was obtained though automatic mean of 64 scans.First derivative spectrum preprocessing method was used,and spectral region(9 750.7~7 498.2 cm-1)was selected to develop mathematical models by partial least square method for nicotinamide tablets samples.Results The optimal rank and mean square error determined for samples though automatic mean of 64 scans by cross validation method were 4 and 3.34 respectively;the average recovery was 99.56%;and the RSD was 2.58%.To verify that the NIR method was feasible for application,the predicted values were compared to the observed values measured by HPLC which was used as the reference method.The paired t-test was applied and the results showed that there was no significant difference between the NIR method and the reference methods(P0.05).Conclusion The NIRDRA method was rapid,simple,and noninvasive,and it can be applied to assay for the content of nicotinamide in tablets.

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Available abstract

Objective To develop a near infrared diffuse reflectance analysis(NIRDRA)method for rapid nondestructive quantitative determination of nicotinamide in tablets.Methods All spectra were measured by a Fourier transform spectrometer equipped with a PbS and a InGaAs detector,an external integrating sphere and a fibre-optic probe for reflectance measurements.All samples were scanned from 12 000 cm-1 to 4 000 cm-1,and each spectrum was obtained though automatic mean of 64 scans.First derivative spectrum preprocessing method was used,and spectral region(9 750.7~7 498.2 cm-1)was selected to develop mathematical models by partial least square method for nicotinamide tablets samples.Results The optimal rank and mean square error determined for samples though automatic mean of 64 scans by cross validation method were 4 and 3.34 respectively;the average recovery was 99.56%;and the RSD was 2.58%.To verify that the NIR method was feasible for application,the predicted values were compared to the observed values measured by HPLC which was used as the reference method.The paired t-test was applied and the results showed that there was no significant difference between the NIR method and the reference methods(P0.05).Conclusion The NIRDRA method was rapid,simple,and noninvasive,and it can be applied to assay for the content of nicotinamide in tablets.

Key concepts: Diffuse reflection, Integrating sphere, Diffuse reflectance infrared fourier transform, Nicotinamide, Near-infrared spectroscopy, Analytical Chemistry (journal), Chemistry, Derivative (finance)

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