Method Establishment of Content Determination of Three Toxic Impurities in Glycerophosphorylcholine Raw Materials
- VernacularTitle:甘磷酸胆碱原料药中3种遗传毒性杂质含量测定方法的建立
- Author:
Weiqi ZHANG
1
;
Qian WANG
2
;
Yan HE
1
;
Xueqin WANG
2
Author Information
1. Henan Provincial Food and Drug Evaluation and Inspection Center，Zhengzhou 450000，China
2. Henan Provincial Institute for Food and Drug Control，Zhengzhou 450008，China
- Publication Type:Journal Article
- Keywords:
GC-MS method;
Glycerophosphorylcholine;
Epichlorhydrin;
Glycidyl;
3-chloro-1，2-propanediol
- From:
China Pharmacy
2021;32(21):2631-2634
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE： To establish GC-MS method for the content determination of three toxic impurities in glycerophosphorylcholine raw materials ，such as epichlorohydrin ，glycidyl，3-chloro-1，2-propanediol. METHODS ：Four batches of glycerophosphorylcholine raw materials were used as test samples. The determination was performed on ZB-WAXplus TM column， and the injector temperature was 200 ℃；the sample injection adopted splitless injection mode ，using helium （He）as carrier gas ， in constant current mode ；the temperature program for the column was initially heating at 30 ℃ for 1 min，rising to 220 ℃ at a speed of 30 ℃/min then remaining 5 min. The ion source was electrospray ion source （EI），the ion source temperature was 200 ℃，and the ionization energy was 70 eV；transmission interface temperature was 250 ℃，and mass spectrum monitoring mode was selected ion （SIM）. Detection ions were epichlorhydrin [mass charge ratio （m/z）49，57，62]，glycidyl（m/z 31，43，44）， 3-chloro-1，2-propanediol（m/z 44，61，79）. The solvent delay time was 3 min. RESULTS ：The linear range of epichlorhydrin ， glycidyl and 3-chloro-1，2-propanediol were 29.86-746.48，172.91-922.18，21.18-211.85 ng/mL，respectively（all r＞0.999 0）. The detection limits were 19.91，115.27，10.59 ng/mL，respectively. The limits of quantitation were 29.86，172.91，21.18 ng/mL， respectively. RSDs of precision （n＝6），reproducibility （n＝6） and stability （placed at room temperature for 12 h，n＝8） tests were all lower than 10％. The average recoveries were 93.88％，91.45％，91.86％，and RSDs were 5.10％，3.10％，2.49％ （n＝9），respectively. In the 4 batches of glycerophosphorylcholine raw materials ，three toxic impurities were all not detected. CONCLUSIONS：Established GC-MS method is simple ，efficient，accurate and repeatable ，and it can be used to determine the contents of three toxic impurities in glycerophosphorylcholine raw materials ，such as epichlorohydrin ，glycidyl，3-chloro-1， 2-propanediol.
