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
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