聚山梨酯类化合物定性鉴别方法研究

Qualitative identification of polysorbate compounds

目的:建立聚山梨酯类化合物的核磁共振和基质辅助激光解吸电离飞行时间质谱(MALDI-TOFMS)定性鉴别方法。方法:核磁共振方法采用5 mm BBO探头的核磁共振仪在温度25℃下,采集一维氢谱和碳谱。一维氢谱弛豫时间2s,谱宽δ_H 15,采样点数64k,扫描次数128次;一维碳谱弛豫时间1S,谱宽δ_C 236.6,采样点数64k,扫描次数32 768次。MALDI-TOF-MS方法采用MALDI-TOF-MS质谱仪,采样基质α-氰基-4-羟基肉桂酸(CHCA),采样质量范围m/z 500~4 000。结果:MALDI-TOF-MS质谱图中的特征离子峰可有效定性鉴别聚山梨酯20、40和60。核磁共振~1H谱、^(13)C谱中的双键信号峰可有效定性鉴别聚山梨酯80。结论:MALDI-TOF-MS法和核磁共振~1H谱、^(13)C谱的结合使用可有效定性鉴别聚山梨酯类化合物。

Objective： To establish a method for the identification of polysorbates using nuclear magnetic resonance （ NMR ） and matrix-assisted laser desorption/ionization time of flight mass spectrometry （ MALDI-TOF-MS ）. Methods： NMR： 1H-NMR and 13C-NMR spectra were collected at Bruker Ascend 500 spectrometer with 5 mm BBO probe at 25℃. In 1D 1H-NMR spectra, the D1 was 2 s, SW was 8 n 15, data point was 64 k and number of scan was 128. In 1D 13C-NMR spectra, the D1 was 1s, SW was δc 236. 6, data point was 64 k and number of scan was 32768. MALDI-TOF-MS： CHCA matrix was adopted, and mass range was m/z 500-4 000. Results： The characteristic ion peaks in the MALDI-TOF-MS spectra were useful for the qualitative identification of polysorbate 20, 40 and 60. Polysorbate 80 was identified by 1H-NMR and 13C-NMR spectra. Conclusion： The combination of 1D IH, 13C-NMR spectra and MALDI-TOF-MS is a specific, simple and convenient method for the qualitative identification of polysorbates.