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目的建立毛细管气相色谱法测定抗病毒原料药恩替卡韦中的有机溶剂残留量。方法采用DB-624毛细管色谱柱,FID检测器。载气为N2,流速为2 ml.min-1,进样口温度250℃,检测器温度为250℃。结果甲醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、三乙胺、甲苯和苯甲醇的线性范围分别为0.060 18～0.601 8 g.L-1(r=0.997 3)、0.012 02～0.120 2 g.L-1(r=0.996 8)、0.005 78～0.057 8 g.L-1(r=0.997 2)、0.103 48～1.034 8 g.L-1(r=0.997 2)、0.017 06～0.170 6 g.L-1(r=0.996 8)、0.101 26～1.012 6 g.L-1(r=0.995 7)、0.018 06～0.180 6 g.L-1(r=0.998 3)和0.100 74～1.007 4 g.L-1(r=0.999 3);平均回收率(n=9)分别为98.6%(RSD=2.36%)、95.5%(RSD=5.98%)、96.9%(RSD=4.36%)、100.5%(RSD=2.02%)、102.3%(RSD=3.86%)、100.1%(RSD=1.56%)、102.4%(RSD=1.88%)、99.4%(RSD=1.63%)。结论该方法操作简便、准确、灵敏度高、重复性好,适用于恩替卡韦原料药中有机溶剂残留量的测定。
OBJECTIVE To establish a capillary gas chromatographic method for the determination of residual organic solvents in the antiviral drug entecavir. Methods DB-624 capillary column and FID detector were used. The carrier gas was N2, the flow rate was 2 ml.min-1, the inlet temperature was 250 ° C, and the detector temperature was 250 ° C. Results The linear ranges of methanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, triethylamine, toluene and benzyl alcohol were 0.060 18-0.60181 gL-1 (r = 0.997 3), 0.012 02-0.120 2 gL (R = 0.9976), 0.00578-0.05708 gL-1 (r = 0.9972), 0.10348-1.0348 gL-1 (r = 0.9972) and 0.017 06-0.1706 gL-1 (r = 0.996 8), 0.101 26-1.012 6 gL-1 (r = 0.995 7), 0.018 06-0.180 6 gL-1 (r = 0.998 3) and 0.100 74-1.007 4 gL-1 (r = 0.999 3) (RSD = 2.36%), 95.5% (RSD = 5.98%), 96.9% (RSD = 4.36%), 100.5% (RSD = 2.02%) and 102.3% (RSD = 3.86%), 100.1% (RSD = 1.56%), 102.4% (RSD = 1.88%), 99.4% (RSD = 1.63%). Conclusion The method is simple, accurate, sensitive and reproducible. It is suitable for the determination of residual organic solvents in entecavir APIs.