Objective: To develop an ultra-high performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q TOF MS) approach to investigate the molecular weight distribution and n value of nonoxynol oligomers, and to study several batches of samples produced domestically or abroad. Methods: The mobile phase was 0.1% trifluoroacetic acid aqueous solution(A)-0.1% trifluoroacetic acid in acetonitrile(B) with linear gradient elution at a flow rate of 0.3 mL·min-1. The column was Techmate STV SUNSHELL Peptide C18(100 mm×2.1 mm, 2.6 μm, 300 ) and installed in a 60 ℃ column oven. Injection volume was 5 μL. A tandem quadrupole time-of-flight mass spectrometer with Dual ESI as ion source and argon as collision gas were used for detection in positive ion mode with a collection range of m/z 50-3 000. ChemDraw 19.0 software was used to draw the relevant structure, and MassHunter PCDL Manager software was used to build the database and edit the calculation formula. Results: The weight average molecular weight and number average molecular weight of 6 batches nonoxynol drug substance produced domestically or abroad were determined by the newly established method, and the range of n average value in the structure was obtained. The results showed that the weight average molecular weight and number average molecular weight were different between domestic and foreign products and also between different batches produced by same manufacturer. The n value of structure basis also varies. The weight average molecular weight ranges were 664.6 to 686.8 (n value was about 10), and number average molecular weight ranges were 677.1 to 715.5 (n value was about 11). Conclusion: The molecular weight distribution and n value of such oligomer drugs need to be controlled in the production process and quality specifications. The newly established method has high sensitivity, precision and reproducibility, can be qualified for the needs of determining molecular weight distribution and n value of nonoxynol, and provides insight in determination of molecular weight distribution of such oligomers. This study also provides a data supplement for the improvement and revision of the standards of Chinese Pharmacopoeia.
ZHANG Wei
,
ZHANG Hui
,
HAN Zhi-guo
,
SUN Ming-hui
,
LIANG Cheng-gang1**
. Molecular weight distribution and n value of nonoxynol were determined by ultra-high performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry*[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(10)
: 1807
-1815
.
DOI: 10.16155/j.0254-1793.2024-0130
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