摘要
目的:建立同时测定阿哌沙班原料中12种残留溶剂的气相色谱法。方法:色谱柱以100%二甲基聚硅氧烷为固定液的HP-1型毛细管柱(30m×0.530mm×2.65μm),载气为氮气,采用程序升温方式,流速为2.8ml/min,进样量为1ml,进样口温度为250℃,检测器为FID检测器,检测器温度为250℃,分流比为5:1。样品瓶平衡温度为100℃,定量环温度为110℃,传输线温度为120℃,样品瓶平衡时间为20min,氢气流量为40ml/min,空气流量为400ml/min,尾吹气25ml/min。结果:在选定的实验方法下,空白溶剂对检测无干扰,且各溶剂峰之间分离度均符合要求。甲醇、乙醇、乙腈、二氯甲烷、乙酸乙酯、四氢呋喃、三乙胺、正庚烷、吡啶、DMF、吗啉、DMSO分别在LOQ~150%线性范围内线性关系良好,定量限在0.29~6.9μg/ml之间,检测限在0.087~2.0μg/ml之间,重复性实验的RSD均小于2%,回收率的平均值在98.0%~102.5%之间。结论:该方法检测简便、专属性强、检测灵敏度高、各溶剂之间分离效果好,可同时用于阿哌沙班原料中12种残留溶剂的测定。
Objective:A gas chromatography method for simultaneous determination of 12 residual solvents in apixaban was established.Method:Chromatographic Column HP-1 capillary column with 100%dimethylpolysiloxane as fixed solution(30m×0.530mm×2.65μm),the carrier gas is nitrogen,using temperature programmed method,the flow rate is 2.8 ml/min,the injection volume is 1ml,the injector temperature is 250℃,the detector is FID detector,the detector temperature is 250℃,and the split ratio is 5:1.The equilibrium temperature of the sample bottle is 100℃,the temperature of the quantitative ring is 110℃,and the temperature of the transmission line is 120℃,the balance time of the sample bottle is 20 min,the hydrogen flow was 40 mL/min,the air flow was 400 mL/min,and the tail air was 25 mL/min.Results:Under the selected experimental method,the blank solvent has no interference to the detection,and the resolution between the solvent peaks meets the requirements.Methanol、ethanol、aceto nitrile、dichloromethane、ethyl acetate、tetrahydrofuran、triethylamine、n-heptane、pyridine、DMF、morpholine and DMSO have good linear relationship in the linear range of LOQ~150%,and the quantitative limit is 0.29~6.9μg/ml,the detection limit is 0.087~2.0 mg/ml,the RSD of the repeatability experiment was less than 2%,and the average recovery was 98.0%~102.5%.Conclusion:The method has the advantages of simple detection,strong specificity,high detection sensitivity and good separation effect between solvents.It can be used for the determination of 12 residual solvents in apixaban raw materials at the same time.
作者
陈俊泽
杨安妮
黄秀梅
Chen Junze;Yang Anni;Huang Xiumei(Zhejiang Yongning Pharmaceutical Co.,Ltd.,Zhejiang,318020)
出处
《当代化工研究》
2022年第16期38-40,共3页
Modern Chemical Research
关键词
阿哌沙班
原料药
顶空气相法
残留溶剂
apixaban
active pharmaceutical ingredients
headspace gas phase method
residual solvents
