Merckle P, Kovar K A
Pharmazeutisches Institut der Universität Tübingen, Germany.
J Pharm Biomed Anal. 1998 Jul;17(3):365-74. doi: 10.1016/s0731-7085(97)00194-5.
Near-infrared spectroscopy (NIRS) was used to determine acetylsalicylic acid (ASA) in three different effervescent tablet formulations. The nominal ASA concentrations were 14.9% in the single substance formulation (ASA Mono), 17.4% in the combination with ascorbic acid (ASA + C) and 8.7% in the combination with paracetamol and ascorbic acid (ASA Combi). In each case the tablet matrix was composed of seven excipients typical of effervescent tablets. All three formulations were measured as intact tablets in diffuse transmittance and reflectance and as powdered tablets in diffuse reflectance. Calibration was carried out by partial least square (PLS) regression of second derivative spectra. High-performance liquid chromatography (HPLC) was used as the reference method. The relative standard errors of calibration (RSEC) achieved for the three NIR methods were between 1.20 and 2.01% for ASA Mono, between 1.91 and 2.21% for ASA + C and between 2.41 and 4.50% for ASA Combi. The results obtained in transmittance mode were comparable with those obtained in reflectance mode, which is normally used in NIRS. In the test sets of ASA Mono and ASA + C relative root mean square (RRMS) values between 2.21 and 3.13% were obtained. The three NIR methods applied are thus suitable for the quantitative determination of ASA in effervescent tablets and have the advantage over HPLC of being rapid and simply carried out with little sample preparation; they are nondestructive and do not require any environmentally harmful reagents.
近红外光谱法（NIRS）用于测定三种不同泡腾片制剂中的乙酰水杨酸（ASA）。单物质制剂（ASA Mono）中ASA的标称浓度为14.9%，与抗坏血酸组合（ASA + C）中的浓度为17.4%，与对乙酰氨基酚和抗坏血酸组合（ASA Combi）中的浓度为8.7%。在每种情况下，片剂基质均由泡腾片典型的七种辅料组成。所有三种制剂均作为完整片剂以漫透射率和反射率进行测量，并作为粉末状片剂以漫反射率进行测量。通过二阶导数光谱的偏最小二乘（PLS）回归进行校准。高效液相色谱法（HPLC）用作参考方法。三种近红外方法获得的校准相对标准误差（RSEC）对于ASA Mono在1.20%至2.01%之间，对于ASA + C在1.91%至2.21%之间，对于ASA Combi在2.41%至4.50%之间。在透射率模式下获得的结果与在近红外光谱法中通常使用的反射率模式下获得的结果相当。在ASA Mono和ASA + C的测试集中，获得的相对均方根（RRMS）值在2.21%至3.13%之间。因此，所应用的三种近红外方法适用于泡腾片中ASA的定量测定，并且相对于HPLC具有快速、样品制备简单的优点；它们是非破坏性的，不需要任何对环境有害的试剂。
