目的 建立气相色谱法测定盐酸托哌酮的残留溶剂的方法。方法 采用气相色谱仪,Agilent 7697A顶空进样器。色谱柱为DB-624（30 m×3.2 mm,1.8 µm）;载气为氮气;燃气为氢气、空气;分流比20∶1;流速2 mL/min;检测器为FID,温度250℃;进样口温度200℃。顶空条件：平衡温度90℃,定量环温度100℃,传输线温度110℃,顶空平衡时间30 min,循环时间35 min。升温程序：40℃保持8 min,以10℃/min升至155℃,保持4 min。结果 检测的五种溶剂回收率均在90%~110%,相对标准偏差≤3.0%。乙醇与丙酮、丙酮与异丙醇、异丙醇与异丙醚、异丙醚与甲苯的分离度分别为6.5、2.3、14.0、60.3。五种物质在检测范围中线性相关系数r≥0.9950。结论 本法可以简单、准确、重复地测定盐酸托哌酮的残留溶剂。

Objective To establish a gas chromatography method for the determination of residual solvent of topazone hydrochloride. Methods The analysis was conducted using a gas chromatograph with an Agilent 7697A headspace sampler and a DB-624 capillary column (30 m×3.2 mm, 1.8 µm). Nitrogen was used as the carrier gas, and hydrogen and air served as fuel gases. The split ratio was set at 20∶1 with a flow rate of 2 ml/min. The temperatures for the FID detector and inlet were maintained at 250℃ and 200℃, respectively. Regarding headspace conditions, the equilibrium temperature was 90℃, the loop temperature was 100℃, and the transfer line temperature was 110℃, with an equilibrium time of 30 min and a cycle time of 35 min. The oven temperature program began at 40℃ for 8 min, then increased to 155℃ at a rate of 10℃/min and was held for 4 min. Results The recovery rates for the five target solvents ranged from 90% to 110%, with RSD ≤ 3.0%. The resolutions between ethanol/acetone, acetone/isopropanol, isopropanol/isopropyl ether, and isopropyl ether/toluene were 6.5, 2.3, 14.0, and 60.3, respectively. The linear correlation coefficients (r) for all five substances were ≥0.9950 within the tested concentration range. Conclusion The method is simple, accurate and repeatable to detect the residual solvent of topazone hydrochloride.