气相色谱法测定氧化白藜芦醇中的4种残留溶剂  

Determination of 4 residual solvents in Oxyresveratrol by gas chromatography

作　　者：徐志琴 沈杰 陈子礼 邹永[1] 徐新军[1] XU Zhiqin;SHEN Jie;CHEN Zili;ZOU Yong;XU Xinjun(School of Pharmaceutical Sciences,Sun Yat-Sen University,Guangzhou 510006,China)

机构地区：[1]中山大学药学院

出　　处：《中国药品标准》2019年第5期437-441,共5页Drug Standards of China

基　　金：广州市科技计划项目(201505041557046);中山市引进创新科研团队项目(2015-224)

摘　　要：目的:建立氧化白藜芦醇中叔丁醇、乙醇、乙酸乙酯、乙二醇4种有机溶剂残留量的测定方法。方法:以DB-624弹性石英毛细管柱为色谱柱(30 m×0.32 mm,1.8μm),采用氢火焰离子化检测器,载气为氮气,进样口温度为250℃,检测器温度为300℃,柱温采用程序升温(70℃保持3 min,以30℃ min^-1的速率升温至100℃,保持8 min,然后以30℃ min^-1的速率升温至210℃),流速为3 mL min^-1。以N,N-二甲基甲酰胺为溶剂,进样体积为1μL。结果:4种有机溶剂均能得到很好的分离。叔丁醇、乙醇、乙酸乙酯、乙二醇检测质量浓度线性范围分别为395.28~1482.3μg mL-1(r=0.9999)、398.16~1493.1μg mL^-1(r=0.9999)、395.84~1484.4μg mL^-1(r=0.9999)、53.12~199.2μg mL^-1(r=0.9996);定量限分别为9.88、19.91、19.79、53.12μg mL^-1,检测限分别为3.95、9.95、9.90、19.92μg mL^-1;精密度、重复性和稳定性的RSD均小于5.0%;乙醇、叔丁醇、乙酸乙酯和乙二醇平均回收率(n=9)分别为100.81%、96.72%、99.14%、99.51%,RSD分别为2.93%、3.98%、2.75%、3.34%,且精密度较好。测定样品三批,样品中叔丁醇的残留量分别为0.03%,0.12%和0.02%,乙醇、乙酸乙酯和乙二醇均未被检测到。结论:本文经方法学验证可用于氧化白藜芦醇中4种残留溶剂的分离与测定。Objective:To establish a method for simultaneous determination of 4 residual organic solvents of tert-butanol,ethanol,ethyl acetate and ethylene glycol in Oxyresveratrol.Methods:The test was performed in DB-624(30 m×0.32 mm,1.8μm)capillary chromatography column.The FID detector was used,the carrier gas was nitrogen,the injection temperature was 250℃ and the detector temperature was 300℃.Column temperature is programmed to 70℃ for 3 min,30℃ min^-1 to 100℃,for 8 minutes,then 30℃ min^-1 increase to 210℃.The flow rate was 3 mL min-1.The injection volume was 1μL with N,N-dimethylformamide as the solvent.Results:Four residual solvents were separated well.The linear ranges of the concentration of tert-butanol,ethanol,ethyl acetate and ethylene glycol fell into 395.28-1482.3μg mL^-1(r=0.9999),398.16-1493.1μg mL-1(r=0.9999),395.84-1484.4μg mL^-1(r=0.9999),and 53.12-199.2μg mL-1(r=0.9996)respectively.The limits of quantitation were 9.88,19.91,19.79 and 53.12μg mL^-1 repectively,and the limits of detection were 3.95,9.95,9.90 and 19.92μg mL^-1 respectively.The RSDs of precision,repeatability and stability were all less than 5.0%.The average recoveries of ethanol,tert-butanol,ethyl acetate and ethylene glycol(n=9)were 100.81%,96.72%,99.14%and 99.51%with RSDs as 2.93%,3.98%,2.75%and 3.34%respectively.The residues of tert-butanol in three batches of sample were 0.03%,0.12%and 0.02%respectively.Ethanol,ethyl acetate and ethylene glycol were not detected.Conclusion:The established method was proved to be suitable for the separation and determination of four residual solvents in Oxyresveratrol after validation.

关 键 词：氧化白藜芦醇 残留溶剂 气相色谱法 

分 类 号：R291.2[医药卫生—民族医学]