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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
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| 篇名： | 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 |
| TITLE： | Method Establishment of Content Determination of Three Toxic Impurities in Glycerophosphorylcholine Raw Materials |
| 摘要： | 目的：建立气-质联用（GC-MS）法同时测定甘磷酸胆碱原料药中环氧氯丙烷、缩水甘油、3-氯-1，2-丙二醇等3种遗传毒性杂质的含量。方法：以4批甘磷酸胆碱原料药为检测样品。色谱柱为ZB-WAXplusTM；进样口温度为200℃；进样方式为不分流进样；载气为氦气（He），恒流模式；程序升温为初始温度30℃保持1min，然后以30℃/min的速率升温至220℃并保持5min；进样量为1μL。离子源为电子轰击源（EI），电离电压为70eV，离子源温度为200℃；质谱传输接口温度为250℃；质谱监测模式为选择离子（SIM）；检测特征离子为环氧氯丙烷[质荷比（m/z）49、57、62]、缩水甘油（m/z31、43、44）、3-氯-1，2-丙二醇（m/z44、61、79）；溶剂延迟时间为3min。结果：环氧氯丙烷、缩水甘油、3-氯-1，2-丙二醇检测的质量浓度线性范围分别为29.86～746.48、172.91～922.18、21.18～211.85ng/mL（r均大于0.9990）；检测限分别为19.91、115.27、10.59ng/mL；定量限分别为29.86、172.91、21.18ng/mL；精密度（n＝6）、重复性（n＝6）、稳定性（室温放置12h，n＝8）试验的RSD均小于10％；平均加样回收率分别为93.88％、91.45％、91.86％，RSD分别为5.10％、3.10％、2.49％（n＝9）。在4批甘磷酸胆碱原料药中，均未检出上述3种遗传毒性杂质。结论：建立的GC-MS法简单高效、准确度高、重复性好，可用于同时测定甘磷酸胆碱原料药中环氧氯丙烷、缩水甘油、3-氯-1，2-丙二醇等3种遗传毒性杂质的含量。 |
| 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. |
| 期刊： | 2021年第32卷第21期 |
| 作者： | 张伟奇，王倩，何燕，王雪芹 |
| AUTHORS： | ZHANG Weiqi，WANG Qian，HE Yan，WANG Xueqin |
| 关键字： | 气-质联用法；甘磷酸胆碱；环氧氯丙烷；缩水甘油；3-氯-1，2-丙二醇 |
| KEYWORDS： | GC-MS method ；Glycerophosphorylcholine；Epichlorhydrin；Glycidyl；3-chloro-1，2-propanediol |
| 阅读数： | 261 次 |
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