目的:研究并建立气相色谱(GC)法测定庚酸炔诺酮中游离庚酸的含量。方法:采用HP-FFAP(0.53 mm×30 m, 1.00μm)毛细管色谱柱(固定相为硝基对苯二甲酸改性的聚乙二醇),以氮气为载气,FID检测器,采用程序升温,分流直接进样,标准曲线法...目的:研究并建立气相色谱(GC)法测定庚酸炔诺酮中游离庚酸的含量。方法:采用HP-FFAP(0.53 mm×30 m, 1.00μm)毛细管色谱柱(固定相为硝基对苯二甲酸改性的聚乙二醇),以氮气为载气,FID检测器,采用程序升温,分流直接进样,标准曲线法计算游离庚酸的含量。结果:游离庚酸的检测限为0.49 ng,定量限为2.45 ng,线性范围9.84~118.04μg·mL^(-1)(r=0.999 9),平均回收率(n=3)为98.8%~101.0%(RSD=1.24%),样品中游离庚酸含量分别为0.69%(批号:ALT803730)、0.54%(批号:80703)。结论:本法简单、快速、灵敏、准确,可对庚酸炔诺酮中游离庚酸进行质量控制。展开更多
H 3PW 12O 40/SiO 2(PW/SiO 2) was prepar ed by the sol-gel method and trimethylolpropane tri-heptanoate(TMH ) was synthes ized by trimethylolpropane(TMP) and heptylic acid(HA) in the presence of H 3PW 12O 40/SiO 2.The ...H 3PW 12O 40/SiO 2(PW/SiO 2) was prepar ed by the sol-gel method and trimethylolpropane tri-heptanoate(TMH ) was synthes ized by trimethylolpropane(TMP) and heptylic acid(HA) in the presence of H 3PW 12O 40/SiO 2.The results showed that the catalyst with 50%(mass)PW had good activity and stability.The optimal esterification conditions were as f ollows:n TMP∶n HA=1∶4,2%(mass)PW/SiO 2,reaction temperature 120—200 ℃ and 3 h.The structure of TMH was characterized by GC,IR, 1HNMR spectra and the rate of esterification was up to 95%.展开更多
The synthesis of butyl heptanoate with n butanol and heptanoic acid as reactants and the rare earth solid super acid SO 2- 4/TiO 2/La 3+ as catalyst had been sutdied.The effects of various actors on the reaction were ...The synthesis of butyl heptanoate with n butanol and heptanoic acid as reactants and the rare earth solid super acid SO 2- 4/TiO 2/La 3+ as catalyst had been sutdied.The effects of various actors on the reaction were investigated.The results showed that the appropriate conditions should be:Weight of catalyst is 0.5g(weight of heptanoic acid is 0.2mol);molar ratio of n butanol to heptanoic acid was 1.8∶1;reaction time was 2.0h;dehydrating agent (Toluene) being 15ml.The yield of butyl heptanoate was about 99.2%.展开更多
文摘H 3PW 12O 40/SiO 2(PW/SiO 2) was prepar ed by the sol-gel method and trimethylolpropane tri-heptanoate(TMH ) was synthes ized by trimethylolpropane(TMP) and heptylic acid(HA) in the presence of H 3PW 12O 40/SiO 2.The results showed that the catalyst with 50%(mass)PW had good activity and stability.The optimal esterification conditions were as f ollows:n TMP∶n HA=1∶4,2%(mass)PW/SiO 2,reaction temperature 120—200 ℃ and 3 h.The structure of TMH was characterized by GC,IR, 1HNMR spectra and the rate of esterification was up to 95%.
文摘The synthesis of butyl heptanoate with n butanol and heptanoic acid as reactants and the rare earth solid super acid SO 2- 4/TiO 2/La 3+ as catalyst had been sutdied.The effects of various actors on the reaction were investigated.The results showed that the appropriate conditions should be:Weight of catalyst is 0.5g(weight of heptanoic acid is 0.2mol);molar ratio of n butanol to heptanoic acid was 1.8∶1;reaction time was 2.0h;dehydrating agent (Toluene) being 15ml.The yield of butyl heptanoate was about 99.2%.
