顶空气相色谱法测定苯并三嗪衍生物YABQ的溶剂残留量

Head-space gas chromatography determination of residual solvents in benzene and triazine derivatives YABQ

目的建立顶空气相色谱法测定苯并三嗪衍生物YABQ中3种残留溶剂含量的方法。方法采用DBWAX毛细管色谱柱(0.45 mm×30 mm,0.85μm),程序升温,柱头压为4 psi(1 psi=6.895 k Pa),进样口温度为200℃,FID检测器温度为250℃,顶空进样,平衡温度为70℃,平衡时间为10 min,以DMSO为溶剂,检测残留溶剂的含量。结果丙酮、吡啶和四氢呋喃检测限分别为0.48、0.10、1.76μg/m L,3种残留溶剂均能有效分离,丙酮、吡啶、四氢呋喃线性关系良好(r>0.9996),平均回收率(n=3)分别为102.22%、99.21%、97.87%,RSD分别为0.56%、1.60%、1.09%,丙酮残留量分别为0.0676%、0.0342%、0.0833%,吡啶和四氢呋喃未检出,残留溶剂含量符合药典规定。结论该方法简便、快速、准确,可用于YABQ中残留溶剂的含量测定。

Objective To establish a head-space gas chromatography method for determination of three residual solvents in benzene and triazine derivatives YABQ. Methods DB-WAX capillary column（0.45 mm×30 mm, 0.85 μm） and temperature program were adopted, the stigma pressure was 4 psi（1 psi = 6.895 k Pa）, the inlet temperature was 200℃,the FID detector temperature was 250℃, the head-space equilibrium temperature was 70℃, the equilibrium time was10 min, DMSO was selected as the solvent, the content of residual solvents were detected. Results The results of acetone, pyridine and tetrahydrofuran detection limits were 0.48 μg/m L, 0.10 μg/m L and 1.76μg/m L, three kinds of residual solvents could be separated, a good linear relationship（r〉0.9996） of acetone, pyridine, tetrahydrofuran were showed,the average recoveries（n =3） were 102.22%, 99.21%, 97.87%, the RSD were 0.56%, 1.60%, 1.09%, the residual amount of acetone were 0.0676%, 0.0342%, 0.0833%, pyridine and tetrahydrofuran were undetected, the residual solvent content in line with the pharmacopoeia. Conclusion The method is simple, rapid, accurate, and can be used as a method for the determination YABQ residual solvent.