摘要
目的：建立测定单磷酸阿糖腺苷原料药中乙醇、乙腈、二氯甲烷、乙酸乙酯、吡啶5种残留溶剂的方法。方法：采用顶空进样气相色谱法。色谱柱为AgilentDB-624毛细管柱，程序升温，进样口温度为200℃，检测器为氢火焰离子化检测器，检测温度为250℃，载气为氮气，流速为3ml/min，进样方式为分流进样，分流比为1∶1，顶空平衡温度为100℃，平衡时间为45min，进样量为1ml。按外标法进行定量分析。结果：5种残留溶剂峰分别与相邻峰分离完全。乙醇、乙腈、二氯甲烷、乙酸乙酯、吡啶的检测质量浓度线性范围为24.7～296.3μg/ml（r＝0.9996）、1.9～23.2μg/ml（r＝0.9990）、2.8～33.6μg/ml（r＝0.9980）、24.7～295.9μg/ml（r＝0.9995）、1.0～11.9μg/ml（r＝0.9986）；精密度、重复性试验的RSD≤4.35％；加样回收率分别为102.4％、102.1％、105.5％、100.3％、98.3％，RSD分别为2.0％、3.4％、4.8％、4.8％、4.0％；定量限为0.3044～0.9880μg/ml，检测限为0.1015～0.3293μg/ml。结论：该方法简单、准确、重复性好，可用于单磷酸阿糖腺苷中5种原料药残留溶剂的检测。
OBJECTIVE:To establish a method for the determination of ethanol,acetonitrile,dichloromethane,ethyl acetate,pyridine in vidarabine monophosphate. METHODS:Headspace GC was performed on the column of Agilent DB-624,programmedtemperature,inlet temperature was 200 ℃,the detector was flame ionization detector,detecting temperature was 250 ℃,nitrogenwas carrier gas,flow rate was 3 ml/min,split ratio was 1 ∶1,the top bottles equilibrium temperature was 100 ℃,and equilibriumtime was 45 min,injection volume was 1 ml. external standard was used for quantitative analysis. RESULTS:The peaks of five residualsolvents could be completely separated from the other peaks respectively,The linear rang was 24.7-296.3 μg/ml for ethanol(r=0.999 6)、1.9-23.2 μg/ml for acetonitrile(r=0.999 0),2.8-33.6 μg/ml for dichloromethane(r=0.998 0),24.7-295.9 μg/ml forethyl acetate(r=0.999 5),1.0-11.9 μg/ml for pyridine(r=0.998 6);RSDs of precision and reproducibility tests were lower than4.35%;recoveries were 102.4%(RSD=2.0%,n=9)、102.1%(RSD=3.4%,n=9)、105.5%(RSD=4.8%,n=9)、100.3%(RSD=4.8%,n=9)、98.3%(RSD=4.0%,n=9). The minimum quantifation limit was 0.304 4-0.988 0 μg/ml and the minimum detection limit was0.101 5-0.329 3 μg/ml. CONCLUSIONS:The method is simple,accurate and reproducible,and can be used for the determinationof residual solvents in vidarabine monophosphate.
作者
焦旭雯
陈华
梁蔚阳
JIAO Xuwen;CHEN Hua;LIANG Weiyang(Guangdong Institute for Drug Control,Guangzhou 510180,China)
出处
《中国药房》
CAS
北大核心
2016年第24期3408-3410,共3页
China Pharmacy
基金
广东省医学科学技术研究基金项目(No.A2015256)
广东省食品药品检验检测技术创新专项资金项目(No.2015ZX05)
作者简介
主管药师。研究方向：生化药品检验和药品标准。电话：020-81887684。E-mail：jjxxww17@163.com;通信作者：主任药师。研究方向：生化药品与生物制品检验和药品标准。电话：020-81887684。E-mail：wl-1023@163.com
