El-Gindy Alaa, Attia Khalid Abdel-Salam, Nassar Mohammad Wafaa, Seda Hamed Hamed Abu, Shoeib Maisra Al-Shabrawi
Suez Canal University, Faculty of Pharmacy, Pharmaceutical Analytical Chemistry Department, Ismailia 41522, Egypt.
J AOAC Int. 2012 Jul-Aug;95(4):1035-42. doi: 10.5740/jaoacint.11-301.
Reflectance near-IR (RNIR) spectroscopy was used for the simultaneous determination of chondroitin (CH), glucosamine (GO), and methyl sulfonyl methane (MSM) in tablets. Simple sample preparation was done by grinding, sieving, and compression of the tablets for improving RNIR spectra. Principal component regression and partial least squares (PLS-1 and PLS-2) were successfully applied to quantify the three components in the studied mixture using information included in RNIR spectra in the range of 4350-9100 cm(-1). The calibration model was developed with drug concentration ranges of 14.5-44.2% (w/w) for CH, 18.4-55.3% (w/w) for GO, and 6-18.6% (w/w) for MSM with addition of tablet excipients to the calibration set in the same ratio as in the tested tablets. The calibration models were evaluated by internal validation, cross-validation, and external validation using synthetic and pharmaceutical preparations. The proposed method was applied for analysis of six batches of the pharmaceutical product. The results of the proposed method were compared with the results of the pharmacopoeial method for the same batch of the pharmaceutical product. No significant differences between the results were found. The RNIR method is accurate and precise, and can be used for QC of pharmaceutical products.
采用反射近红外（RNIR）光谱法同时测定片剂中的软骨素（CH）、氨基葡萄糖（GO）和甲基磺酰甲烷（MSM）。通过研磨、筛分和压片进行简单的样品制备，以改善RNIR光谱。主成分回归和偏最小二乘法（PLS - 1和PLS - 2）成功应用于利用4350 - 9100 cm(-1)范围内RNIR光谱中的信息对研究混合物中的三种成分进行定量。校准模型的建立所使用的药物浓度范围为：CH为14.5 - 44.2%（w/w），GO为18.4 - 55.3%（w/w），MSM为6 - 18.6%（w/w），在校准集中添加片剂辅料的比例与测试片剂中的比例相同。校准模型通过使用合成制剂和药物制剂进行内部验证、交叉验证和外部验证来评估。所提出的方法应用于六批药品的分析。将所提出方法的结果与同一批药品的药典方法结果进行比较。结果之间未发现显著差异。RNIR方法准确、精密，可用于药品的质量控制。
