顶空气相色谱法同时测定艾司奥美拉唑镁原料药中6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艾司奥美拉唑镁原料药中6种有机溶剂的残留量
TITLE:
摘要: 目的:建立同时测定艾司奥美拉唑镁原料药中甲醇、异丙醇、乙腈、二氯甲烷、乙酸乙酯、甲苯6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DB-624毛细管柱,程序升温,进样口温度为200 ℃,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,氮气流速为2.0 mL/min,分流比为5 ∶ 1,顶空进样量为1 mL,顶空平衡温度为80 ℃,平衡时间为20 min。结果:甲醇、异丙醇、乙腈、二氯甲烷、乙酸乙酯、甲苯检测质量浓度线性范围分别为12.56~628.00 μg/mL(r=0.999 7)、20.22~1 011.20 μg/mL(r=0.999 9)、1.96~97.76 μg/mL(r=0.999 7)、3.10~154.88 μg/mL(r=0.999 8)、20.69~1 034.56 μg/mL(r=0.999 8)、3.53~176.72 μg/mL(r=0.999 8);定量限分别为1.00、0.91、0.47、0.93、0.41、0.35 μg/mL,检测限分别为0.31、0.30、0.14、0.31、0.12、0.11 μg/mL;精密度、稳定性、重复性试验的RSD<3%;加样回收率分别为94.53%~101.29%(RSD=2.15%,n=9)、97.78%~103.42%(RSD=1.77%,n=9)、96.99%~105.76%(RSD=2.59%,n=9)、96.83%~102.05%(RSD=1.86%,n=9)、97.98%~101.13%(RSD=0.88%,n=9)、97.80%~102.40%(RSD=1.41%,n=9)。结论:该方法灵敏、准确,可用于艾司奥美拉唑镁原料药中甲醇、异丙醇、乙腈、二氯甲烷、乙酸乙酯、甲苯6种有机溶剂残留量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for the simultaneous determination of 6 kinds of residual organic solvents in Omeprazole magnesium, such as methanol, isopropanol, acetonitrile,dichloromethane, ethyl acetate and toluenein. METHODS: Headspace GC was adopted. The determination was performed on the column of DB-624 column by temperature programming. The inlet temperature was 200 ℃, and hydrogen flame ionization detector was adopted with the temperature of 250 ℃; nitrogen gas was used as carrier gas with flow rate of 2.0 mL/min; the splitting-radio was 5 ∶ 1, and sample size was 1 mL; the headspace temperature was 80 ℃ and the equilibrium time was 20 min. RESULTS: The linear range were 12.56-628.00 μg/mL for methanol (r=0.999 7), 20.22-1011.20 μg/mL for isopropanol (r=0.999 9), 1.96-97.76 μg/mL for acetonitrile (r=0.999 7),3.10-154.88 μg/mL for dichloromethane (r=0.999 8),20.69-1034.56 μg/mL for ethyl acetate (r=0.999 8), and 3.53-176.72 μg/mL for toluene (r=0.999 8); the limits of quantitation were 1.00, 0.91, 0.47, 0.93, 0.41 and 0.35 μg/mL respectively; the limits of detection were 0.31, 0.30, 0.14, 0.31, 0.12 and 0.11 μg/mL respectively; RSDs of precision, stability and reproducibility tests were lower than 3%; the recoveries were 94.53%-101.29% (RSD=2.15%,n=9), 97.78%-103.42% (RSD=1.77%,n=9), 96.99%-105.76% (RSD=2.59%,n=9), 96.83%-102.05% (RSD=1.86%,n=9), 97.98%-101.13%(RSD=0.88%,n=9) and 97.80%-102.40% (RSD=1.41%,n=9). CONCLUSIONS: The method is sensitive and accurate, can be used for the simultaneous determination of 6 kinds of residual organic solvents in Omeprazole magnesium, such as methanol, isopropanol, acetonitrile, dichloromethane, ethyl acetate and toluenein.
期刊: 2017年第28卷第15期
作者: 姜鹰雁,耿志鹏,刘燕,索栋,杨海霞
AUTHORS: JIANG Yingyan,GENG Zhipeng,LIU Yan,SUO Dong,YANG Haixia
关键字: 艾司奥美拉唑镁;顶空气相色谱法;有机溶剂;残留量;甲醇;异丙醇;乙腈;二氯甲烷;乙酸乙酯;甲苯
KEYWORDS: Omeprazole magnesium; Headspace GC; Organic solvent; Residual; Methanol; Isopropanol; Acetonitrile; Dichloromethane; Ethyl acetate; Toluenein
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