顶空气相色谱法同时测定硫酸沃拉帕沙原料药中7种有机溶剂的残留量
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篇名: 顶空气相色谱法同时测定硫酸沃拉帕沙原料药中7种有机溶剂的残留量
TITLE:
摘要: 目的:建立同时测定硫酸沃拉帕沙原料药中7种有机溶剂残留量的方法。方法:采用顶空气相色谱法。色谱柱为Agilent DB-624毛细管柱,程序升温,进样口温度为220 ℃,检测器为氢火焰离子化检测器,检测器温度为250 ℃,载气为氮气(纯度:99.999%),流速为2.0 mL/min,分流比为20 ∶ 1,顶空进样量为1 mL,顶空平衡温度为80 ℃,顶空平衡时间为30 min。结果:乙酸乙酯、甲醇、二氯甲烷、乙醇、乙腈、四氢呋喃、甲苯检测质量浓度线性范围分别为2.0~201.0 μg/mL(r=0.999 8)、1.2~122.3 μg/mL(r=0.999 4)、0.24~24.0 μg/mL(r=0.999 2)、2.0~200.3 μg/mL(r=0.999 9)、0.2~16.7 μg/mL(r=0.999 9)、0.3~29.0 μg/mL(r=0.999 3)、0.4~35.8 μg/mL(r=0.999 3);定量限分别为2.0、1.2、0.24、2.0、0.2、0.3、0.4 μg/mL,检出限分别为0.60、0.30、0.07、0.60、0.06、0.09、0.12 μg/mL;精密度、稳定性、重复性试验的RSD均小于4%;加样回收率分别为97.02%~99.84%(RSD=0.88%,n=9)、98.05%~99.64%(RSD=0.54%,n=9)、97.37%~100.00%(RSD=0.83%,n=9)、98.67%~99.60%(RSD=0.34%,n=9)、 97.56%~99.76%(RSD=0.79%,n=9)、97.22%~99.45%(RSD=0.65%,n=9)、97.75%~99.33%(RSD=0.59%,n=9);耐用性试验的RSD均小于8%。原料药样品中仅检出甲醇、乙醇。结论:该方法操作简便、准确,精密度、稳定性、重复性、耐用性好,可用于硫酸沃拉帕沙原料药中7种有机溶剂残留量的同时测定。
ABSTRACT: OBJECTIVE: To establish simultaneous determination of 7 kinds of residual solvents in vorapaxar sulfate raw material. METHODS: The headspace gas chromatography was performed on Agilent DB-624 capillary column(programmed temperature) with inlet temperature of 220 ℃, detection temperature of 250 ℃ using nitrogen(99.999%) as carrier gas at the flow rate of 2.0 mL/min. The split ratio was 20 ∶ 1, and sample size was 1 mL. The headspace equilibrium temperature was 80 ℃,headspace equilibrium time was 30 min. RESULTS: The linear range of ethyl acetate, methanol, dichloromethane, ethanol, acetonitrile, tetrahydrofuran and toluene were 2.0-201.0 μg/mL(r=0.999 8), 1.2-122.3 μg/mL(r=0.999 4), 0.24-24.0 μg/mL(r=0.999 2), 2.0-200.3 μg/mL(r=0.999 9), 0.2-16.7 μg/mL(r=0.999 9), 0.3-29.0 μg/mL(r=0.999 3), 0.4-35.8 μg/mL(r=0.999 3), respectively. The limits of quantification were 2.0, 1.2, 0.24, 2.0, 0.2, 0.3, 0.4 μg/mL; the limits of detection were 0.60, 0.30, 0.07, 0.60, 0.06, 0.09, 0.12 μg/mL. RSDs of precision, stability and reproducibility tests were all lower than 4%. The recoveries were 97.02%-99.84%(RSD=0.88%,n=9), 98.05%-99.64%(RSD=0.54%,n=9), 97.37%-100.00%(RSD=0.83%,n=9), 98.67%-99.60%(RSD=0.34%,n=9), 97.56%-99.76%(RSD=0.79%,n=9), 97.22%-99.45%(RSD=0.65%,n=9), 97.75%-99.33%(RSD=0.59%,n=9), respectively. RSDs of durability tests were all lower than 8%. Methanol, ethanol were detected in samples. CONCLUSIONS: The method is simple, accurate, precise, stable, reproducible and durable, and can be used for simultaneous determination of 7 kinds of residual solvents in vorapaxar sulfate raw material.
期刊: 2018年第29卷第16期
作者: 刘英,刘葵葵,邓玉晓,孙德清
AUTHORS: LIU Ying,LIU Kuikui,DENG Yuxiao,SUN Deqing
关键字: 顶空气相色谱法;硫酸沃拉帕沙;残留溶剂
KEYWORDS: Headspace gas chromatography; Vorapaxar sulfate; Residual solvents
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