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頂空氣相色譜法測定鹽酸普拉克索中的溶劑殘留量

發(fā)布時間:2018-09-19 20:42
【摘要】:目的建立頂空氣相色譜法測定鹽酸普拉克索中有機溶劑殘留量的方法。方法采用Agilent DB-624(30 m×0.25mm,1.4μm)毛細(xì)管柱,氮氣為載氣,程序升溫,氫離子火焰檢測器,測定鹽酸普拉克索中甲醇、異丙醇、乙酸乙酯和四氫呋喃的溶劑殘留量。結(jié)果甲醇、異丙醇、乙酸乙酯及四氫呋喃色譜峰均能得到有效分離,且質(zhì)量濃度分別在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內(nèi)與峰面積呈良好線性關(guān)系(r≥0.999 0),平均回收率在93.3%~108.6%內(nèi);甲醇、異丙醇、乙酸乙酯和四氫呋喃的檢測限分別為0.91、0.6、0.33和0.44 mg·L-1,定量限分別為3.64、2.4、1.33和1.75mg·L-1。結(jié)論本方法靈敏、準(zhǔn)確、可靠,可用于鹽酸普拉克索中殘留溶劑的測定。
[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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