重定向消息
获取报价

药用多肽的自动水分分析

AN-NIR-078

2020-01

zh

Non-destructive quality control

冻干药用多肽中残留水分的定量分析是制药行业质量控制的一项重要措施。出于开发目的，在稳定性研究和优化冻干工艺（冻干）过程中，此类测量是需要和常规的。目前，卡尔费休滴定法被广泛用于常规分析中的水分测定。然而，这种方法耗时较长，而且在分析过程中会破坏样品。本应用说明介绍了近红外光谱 (NIRS) 是一种快速、无试剂、非破坏性的方法，可用于测定冻干药品中的水分含量。

The quantification of residual moisture in lyophilized pharmaceutical peptides is an important measure for quality control in the pharmaceutical industry. Analyses are routinely performed for process control and to ensure that production lots meet required specifications. For development purposes, such measurements are necessary during stability studies and to optimize the freeze-drying process (lyophilization).

Currently, Karl Fischer titration is widely used for moisture determination in routine analysis. However, measuring the water content by this method is time consuming and the sample is destroyed during analysis. This Application Note shows that near-infrared spectroscopy (NIRS) is a fast, reagentless, non destructive method to determine moisture content in lyophilized pharmaceutical products.

Figure 1. The NIRS XDS OptiProbe Analyzer and the 815 Robotic Sample Processor.

17 spectra of samples with varying moisture content were collected using a Metrohm NIRS XDS OptiProbe Analyzer in combination with the 815 Robotic Sample Processor. With the attached large sample rack, it was possible to automate measurements of up to 62 samples in series. The reference values were obtained by KF-titration. The data set consisting of spectra and lab values was split into a calibration set (11 samples) and validation set (6 samples). Outlier detection was performed on pre-treated spectra (2nd derivative) using a maximum distance in wavelength space algorithm.

Pre-processing Algorithm Validation type
2nd derivative PLS Independent validation set
Figure 2. Protein samples measured with varying water content.

The obtained correlation graph displays a very high correlation (R2 = 0.99) between moisture predicted by NIRS and the KF-titration primary method. SEC and SEV values are in the range of 0.060%, which proves that NIRS is a sensitive and suitable technique for moisture determination.

# Factors R2 SEC SEV
2 0.99 0.054% 0.061%
Figure 3. Correlation graph for moisture predicted by NIRS vs titration.
咨询

瑞士万通中国

北京市海淀区上地东路1号院1号楼7层702
100085 北京

咨询