摘要
目的 建立气相色谱法测定氟比洛芬酯中的1-氯乙基乙酸酯。方法 使用DB-1毛细管色谱柱(30 m×0.32 mm,1.0μm),升温程序:起始温度为80℃,维持2 min,以5℃·min-1的速率升至100℃,维持4 min。FID检测器温度:250℃;进样口温度:200℃;载气:高纯氮气,载气流速:1 mL·min^(-1),进样量为1μL。结果 1-氯乙基乙酸酯在0.61~9.08μg·mL^(-1)范围内,回归方程为y=0.919x+0.046 7(r=0.999 4)。1-氯乙基乙酸酯的回收率在98.89%~109.35%之间,平均回收率为102.8%(RSD为3.4%)。精密度、定量限、检测限、溶液稳定性、耐用性经验证,结果均良好。1-氯乙基乙酸酯为制备氟比洛芬酯的中间体,精制前的氟比洛芬酯中,1-氯乙基乙酸酯的含量远远小于限度。精制后的氟比洛芬酯,均未检出1-氯乙基乙酸酯。结论 本方法操作简便,重复性好,灵敏度高,能满足测定氟比洛芬酯中1-氯乙基乙酸酯的要求。
OBJECTIVE To establish gas chromatography method for the determination of impurity-1-chloroethyl acetate in flurbiprofen axe til.METHODS The method was performed on a capillary chromatographic column(DB-1 30 m×0.32 mm,1.00 μm).The programmed temperature was applied:The column temperature was 80 ℃(maintained for 2 min),then raised to 100 ℃(maintained for 4 min) at the rate of 5 ℃·min^(-1).FID was used as detector at the temperature of 250 ℃ with the inlet temperature seting at 200 ℃.Carrier gas was nitrogen with a flow rate of 1 mL·min^(-1).The injection volume was 1 μL.RESULTS The linearity regression equation of 1-chloroethyl acetate was y=0.919 x+0.046 7(r=0.999 4) in the range of 0.61-9.08 μg·mL^(-1).The recovery ranged from 98.89% to 109.35%,with an average recovery of 102.8%(RSD=3.4%).Precision,quantitative limit,detection limit,stability of the solution,durability tests had been verified with good results.1-Chloroethyl acetate was an intermediate in producing flurbiprofen axe til,whose content was much less than the limit in the unpurified flurbiprofen are til.Besides,1-chloroethyl acetate was not detected in purified flurbiprofen axetil.CONCLUSION The method is simple to operate with good reproducibility and high sensitivity,which meet the requirements for the determination of chloroethanol acetate in flulbeprofen axe til.
作者
谢春燕
鲁丹
曾少群
岳峰
XIE Chunyan;LU Dan;ZENG Shaoqun;YUE Feng(Guangdong Jiabo Pharmaceutical Co.,Ltd.,Qingyuan,Guangdong 511517,China;Guangdong Engineering Center of Intravenous Lipid Emulsion,Qingyuan,Guangdong 511517,China)
出处
《今日药学》
CAS
2022年第5期363-368,共6页
Pharmacy Today
基金
清远市科技计划项目(2019DZX003)
广东省科技发展专项资金项目(2017B010136137)。
