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目的::建立丹酚酸B原料药中3种残留溶剂的测定方法。方法:采用顶空毛细管气相色谱法测定,色谱柱为HP-5毛细管柱(30 m ×0.32 mm,0.6μm),进样口温度为180℃,进样量为0.1 ml,分流比为1∶10;柱温为40℃保持6 min,15℃· min-1升温至180℃,保持5 min;检测器为FID,温度:250℃;载气:N2,流速:1.7 ml·min-1。二甲亚砜(DMSO)为溶剂。结果:各残留溶剂均可达到基线分离。各残留溶剂乙醇、丙酮和乙酸乙酯分别在12.650~1.012×103μg·ml-1(r =0.9993)、12.750~1.020×103μg·ml-1(r=0.9997)、12.550~1.004×103μg·ml-1(r=0.9997)范围内线性关系良好。乙醇、丙酮、乙酸乙酯的平均回收率分别为96.89%(RSD=3.81%,n=9)、99.56%(RSD=4.05%,n=9)、97.21%(RSD=4.95%,n=9)。结论:该法操作简便,重复性好,结果准确可靠,可以用于丹酚酸B原料药中残留溶剂的测定。“,”Objective:To establish a method to determine the residual solvents in salvianolic acid B. Methods: The headspace GC was carried out on an HP-5 capillary column(30 m × 0. 32 mm,0. 6 μm). The inlet temperature was 180℃. The injection volume was 0. 1ml and the separation ratio was 1:10. The column temperature was programmed:the initial temperature was 40℃, malntalned for 6 min, ralsed to 180℃ with a rate of 15 ℃·min-1 , and malntalned for another 5 min. The detector was FID with the temperature of 250℃. The carrier gas was N2 with the flow rate of 1. 7 ml·min-1 . DMSO was used as the solvent for salvianolic acid B. Results:All solvents could be separated completely. The linear range of ethanol, acetone and ethyl acetate was 12. 650-1. 012 × 103 μg·ml-1 (r=0.999 3),12.750-1.012 ×103 μg·ml-1(r=0.999 7) and 12.550-1.004 ×103 μg·ml-1(r=0.999 7), respectively. The average recovery of ethanol, acetone and ethyl acetate was 96. 89% (RSD=3. 81%,n=9), 99. 56% (RSD=4. 05%,n=9) and 97. 21% (RSD=4. 95%,n=9), respectively. Conclusion:The method is simple, reproducible and accurate enough for the determi-nation of residual solvents in salvianolic acid B.