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  

Determination of 9 Residual Organic Solvents in Blonanserin by Headspace Gas Chromatography

作　　者：裴丽娟[1] 田晨[1] 齐然然 张卓[1] 王业[1] 

机构地区：[1]河北医科大学第一医院药剂科,石家庄050031

出　　处：《中国药房》2017年第12期1699-1702,共4页China Pharmacy

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 m L/min,分流比为1∶1,顶空进样量为1 m L,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 500μg/m L(r=0.999 8)、10~2 500μg/m L(r=0.999 9)、10~2 500μg/m L(r=0.999 8)、0.82~205μg/m L(r=0.999 4)、1.2~300μg/m L(r=0.999 5)、0.58~145μg/m L(r=0.999 4)、10~2 500μg/m L(r=0.999 9)、1.44~360μg/m L(r=0.999 6)、1.78~445μg/m L(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、0.22μg/m L,检测限分别为5.89、1.90、1.05、2.48、0.51、0.23、0.31、0.33、0.07μg/m L;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。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 500μg/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

关 键 词：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 

分 类 号：R927.2[医药卫生—药学]