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目的建立紫杉醇中残留的甲醇、丙酮和正己烷的限量检测方法。方法DB-624毛细管柱(30m×0.53mm×3.0μm);氮气为载气,流速2.0mL·min-1;柱温:60℃保持15分钟,以30℃·min-1的速率升温至180℃,保持5分钟;进样口温度:180℃,分流比5:1;检测器:FID,200℃。顶空进样器:顶空瓶温度85℃,平衡时间30分钟;传输管温度110℃;定量管温度105℃;加压时间0.5min;进样时间1min。结果甲醇、丙酮和正己烷的线性范围分别为:12.00～180.1μg·mL-1(r=0.9996)、1.996～299.5μg·mL-1(r=0.9999)和0.2314～17.36μg·mL-1(r=0.9995);最低检测限分别为2.4μg·mL-1、0.57μg·mL-1和0.048μg·mL-1。结论本方法适合于限量检测紫杉醇中残留的甲醇、丙酮和正己烷。
OBJECTIVE To establish a limit test method for residual methanol, acetone and n-hexane in paclitaxel. Methods Column DB-624 capillary column (30m × 0.53mm × 3.0μm) was used as the carrier gas and the flow rate was 2.0mL · min-1. The column temperature was kept at 60 ℃ for 15 minutes and the temperature was raised to 180 ℃ at a rate of 30 ℃ · min-1 ℃, for 5 minutes; Inlet temperature: 180 ℃, split ratio 5: 1; Detector: FID, 200 ℃. Headspace sampler: headspace bottle temperature 85 ℃, equilibration time 30 minutes; transfer tube temperature 110 ℃; quantitative tube temperature 105 ℃; pressurization time 0.5min; injection time 1min. Results The linear ranges of methanol, acetone and n-hexane were 12.00-180.1 μg · mL -1 (r = 0.9996), 1.996-299.5 μg · mL -1 (r = 0.9999) and 0.2314-17.36 μg · mL -1 r = 0.9995). The limits of detection were 2.4μg · mL-1, 0.57μg · mL-1 and 0.048μg · mL-1, respectively. Conclusion This method is suitable for the limited detection of residual methanol, acetone and n-hexane in paclitaxel.