顶空气相色谱法测定盐酸普拉克索中的溶剂残留量

发布时间：2018-09-19 20:42

【摘要】：目的建立顶空气相色谱法测定盐酸普拉克索中有机溶剂残留量的方法。方法采用Agilent DB-624(30 m×0.25mm,1.4μm)毛细管柱,氮气为载气,程序升温,氢离子火焰检测器,测定盐酸普拉克索中甲醇、异丙醇、乙酸乙酯和四氢呋喃的溶剂残留量。结果甲醇、异丙醇、乙酸乙酯及四氢呋喃色谱峰均能得到有效分离,且质量浓度分别在24.1~96.4mg·L-1、40~160.2mg·L-1、39.9~159.7 mg·L-1和5.8~23.1 mg·L-1内与峰面积呈良好线性关系(r≥0.999 0),平均回收率在93.3%~108.6%内;甲醇、异丙醇、乙酸乙酯和四氢呋喃的检测限分别为0.91、0.6、0.33和0.44 mg·L-1,定量限分别为3.64、2.4、1.33和1.75mg·L-1。结论本方法灵敏、准确、可靠,可用于盐酸普拉克索中残留溶剂的测定。
[Abstract]:Objective to establish a headspace gas chromatography method for the determination of residual organic solvents in Praxol hydrochloride. Methods the solvent residues of methanol, isopropanol, ethyl acetate and tetrahydrofuran in Praxol hydrochloride were determined by Agilent DB-624 capillary column (30 m 脳 0.25 mm ~ (1.4 渭 m), nitrogen as carrier gas, programmed temperature and hydrogen ion flame detector. Results the chromatographic peaks of methanol, isopropanol, ethyl acetate and tetrahydrofuran were effectively separated. The linear relationship between the peak area of methanol, isopropanol, ethyl acetate and tetrahydrofuran was found in the range of 24.1~96.4mg L-1 40160.2mg / L ~ 39.9mg / L ~ 159.7 mg ~ (-1) and 5.823.1 mg ~ (-1) (r 鈮，

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