顶空气相色谱法同时测定布南色林原料药中9种有机溶剂的残留量 点击下载
论文标题: 顶空气相色谱法同时测定布南色林原料药中9种有机溶剂的残留量
英文标题:
中文摘要: 目的:建立同时测定布南色林原料药中甲醇、乙醇、异丙醇、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃和甲苯9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150 ℃,检测器为氢火焰离子化检测器,温度为250 ℃,载气为高纯氮气,载气流速为2.8 mL/min,分流比为1 ∶ 1,顶空进样量为1 mL,顶空加热温度为90 ℃,平衡时间为35 min。结果:甲醇、乙醇、异丙醇、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃和甲苯检测质量浓度线性范围分别为6~1 500 μg/mL(r=0.999 8)、10~2 500 μg/mL(r=0.999 9)、10~2 500 μg/mL(r=0.999 8)、0.82~205 μg/mL(r=0.999 4)、1.2~300 μg/mL(r=0.999 5)、0.58~145 μg/mL(r=0.999 4)、10~2 500 μg/mL(r=0.999 9)、1.44~360 μg/mL(r=0.999 6)、1.78~445 μg/mL(r=0.999 5);定量限分别为17.71、6.02、3.17、7.45、1.53、0.69、0.93、1.01、0.22 μg/mL,检测限分别为5.89、1.90、1.05、2.48、0.51、0.23、0.31、0.33、0.07 μg/mL;精密度、稳定性试验的RSD<3.0%,重复性试验中只检出异丙醇,RSD=2.1%;加样回收率分别为96.67%~102.66%(RSD=1.9%,n=9)、96.00%~101.83%(RSD=1.9%,n=9)、97.17%~101.50%(RSD=1.4%,n=9)、96.97%~102.44%(RSD=2.2%,n=9)、95.83%~103.33%(RSD=2.5%,n=9)、95.83%~100.28%(RSD=1.9%,n=9)、98.17%~101.25%(RSD=1.0%,n=9)、96.55%~102.30%(RSD=1.9%,n=9)、96.30%~102.22%(RSD=1.8%,n=9)。结论:该方法操作简单、快速,结果准确,可用于布南色林原料药中甲醇、乙醇、异丙醇、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃和甲苯9种有机溶剂残留量的同时测定。
英文摘要: OBJECTIVE: To establish a method for the determination of 9 residual organic solvents in blonanserin as methanol, alcohol, isopropyl alcohol, acetonitrile, dichloromethane, hexane, ethyl acetate, tetrahydrofuran and methylbenzene. METHODS: Headspace gas chromatography was adopted. The determination was performed on DB-624 capillary column using temperature programming. The inlet temperature was 150 ℃, and flame ionization detector was used with temperature of 250 ℃. High purity nitrogen was used as carrier gas with flow rate of 2.8 mL/min. The split ratio was 1 ∶ 1, and headspace sample size was 1 mL. Headspace heating temperature was 90 ℃, and equilibration time was 35 min. RESULTS: The linear ranges of methanol, alcohol, isopropyl alcohol, acetonitrile, dichloromethane, hexane, ethyl acetate, tetrahydrofuran and methylbenzene were 6-1 500 μg/mL(r=0.999 8),10-2 500 μg/mL(r=0.999 9),10-2 500 μg/mL(r=0.999 8), 0.82-205 μg/mL(r=0.999 4),1.2-300 μg/mL(r=0.999 5), 0.58-145 μg/mL(r=0.999 4),10-2 500 μg/mL(r=0.999 9),1.44-360 μg/mL(r=0.999 6),1.78-445 μg/mL(r=0.999 5), respectively. The limits of quantitation were 17.71, 6.02, 3.17, 7.45, 1.53, 0.69, 0.93, 1.01, 0.22 μg/mL; the limits of detection were 5.89, 1.90, 1.05, 2.48, 0.51, 0.23, 0.31, 0.33, 0.07 μg/mL, respectively. RSDs of precision and stability tests were all lower than 3.0%, and isopropanol was found in repeatability test (RSD=2.1%). The average recoveries ranged 96.67%-102.66% (RSD=1.9%,n=9),96.00%-101.83%(RSD=1.9%,n=9), 97.17%-101.50%(RSD=1.4%,n=9), 96.97%-102.44%(RSD=2.2%,n=9),95.83%-103.33%(RSD=2.5%,n=9), 95.83%-100.28%(RSD=1.9%,n=9), 98.17%-101.25%(RSD=1.0%,n=9), 96.55%-102.30%(RSD=1.9%,n=9),96.30%-102.22%(RSD=1.8%,n=9), respectively. CONCLUSIONS: The method is simple, rapid, accurate and suitable for simultaneous determination of 9 residual organic solvents in blonanserin as methanol, alcohol, isopropyl alcohol, acetonitrile, dichloromethane, hexane, ethyl acetate, tetrahydrofuran and methylbenzene.
期刊: 2017年第28卷第12期
作者: 裴丽娟,田晨,齐然然,张卓,王业
英文作者: PEI Lijuan,TIAN Chen,QI Ranran,ZHANG Zhuo,WANG Ye
关键字: 布南色林;顶空气相色谱法;残留量;甲醇;乙醇;异丙醇;乙腈;二氯甲烷;正己烷;乙酸乙酯;四氢呋喃;甲苯
KEYWORDS: Blonanserin; Headspace gas chromatography; Residual organic; Methanol; Alcohol; Isopropyl alcohol; Acetonitrile; Dichloromethane; Hexane; Ethyl acetate; Tetrahydrofuran; Methylbenzene
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