热门品牌
Sinaptec NexTgen 系列设备成功应⽤于快速制备⽔基型库仑滴定法(电量滴定) Ultrasound-assisted rapid preparation of water standards for Karl Fischer coulometric titration
快速量化⽔基型库仑滴定法(电量滴定)实验实现省时且可复制性
利⽤ Sinaptec NexTgen 超声设备提供的超声环境和相关溶剂(甲醇和⼆甲基亚砜) 成功实现从酒⽯酸钠⼆⽔化合物中提取⽔,不仅实现可重复性和可复制性,⽽且实现快速制备以达到节约宝贵时间⺫的.
可快速实现对药物,⾷物等含⽔量化测定
Ultrasound-assisted extraction of water from sodium tartrate dihydrate in methanol and DMSO proved to be a reproducible, time-saving method for the preparation of water standards for Karl Fischer titration (KFT)
实验综合结论
与传统样品制备相⽐,超声环境反应下效果明显,省时性和低成本性突出. Significant time and cost savings compared to traditional sample preparation workflows based on
应⽤设备参考
1@SinapTec NexTgen Lab120 1@Sinaptec Probe 1@ Sinaptec Sound Enclosure 1@ Sinaptec Adjustable Platform 1@ Horizontal Shaker
Fig. 2: Ultrasound-assisted preparation of water control standards (complete workflow duration including KF titration: ca. 10-15 min)
Fig. 3: Sodium tartrate dihydrate in methanol. The salt is sparsely soluble in methanol, making it impossible to visually assess if water extraction has been completed.
Fig. 4: Time-course of water extraction from 100 mg sodium tartrate dihydrate in 5mL methanol by ultrasonication (blue) vs. horizontal shaking (red). 3 samples per timepoint were prepared (N=3) and analysed by KF once (n=1). Maximum extraction reaches around 40% of the total hydrate water with this ratio of tartrate/solvent.
Fig. 5: Sodium tartrate dihydrate (100 mg in 5 mL methanol) before (left) and after (right) 30 s of ultrasonic treatment at 70% fixed amplitude. Temperature rises to 42°C after ultrasonication.
Fig. 6: Water control standards prepared in 5mL methanol (Y-axis: ppm i.e. μg /g). 3 samples per concentration were prepared (N=3) and analysed by KF once (n=1).
Fig. 7: Water control standards prepared in 5mL methanol (Y-axis: recovery (%) i.e. actual H2O/ stoichiometric H2O μg/μg)
Fig. 8: Water control standards prepared in 5mL DMSO (Y-axis: ppm i.e. μg /g). 3 samples per concentration were prepared (N=3) and analysed by KF once (n=1). DMSO could be a less toxic alternative solvent to methanol. Its water extraction capacity is comparable to methanol.
Fig. 9: Water control standards prepared in 5mL DMSO (Y-axis: recovery (%) i.e. actual H2O/ stoichiometric H2O μg/μg)
Fig. 10: Water control standards prepared in 5mL ethyl acetate (Y-axis: ppm i.e. μg /g). 3 samples per concentration were prepared (N=3) and analysed by KF once (n=1). Ethyl acetate is a less toxic and less polar solvent than methanol. Its water extraction capacity is very low, however. It is not suitable for the preparation of water standards.
Fig. 11: Ultrasonic power generation with the NexTGen Lab120 homogenizer is highly reproducible: 3 water control standards in methanol are prepared under identical conditions (100 mg sodium tartrate dihydrate per 5 mL methanol. Ultrasonic protocol: fixed amplitude 70%, duration 30 s)
Fig. 12: Reproducibility and stability of 5 water control standards prepared with ultrasonic extraction under identical conditions. 5 samples were prepared (N=5) and analysed by KF three times (n=3).
应⽤学者及⽂献来源信息
Please cite this article Authors:
1.Nenad Gajovic-Eichelmann ,Fraunhofer IZI-BB, Am Mühlenberg 13, 14476 POTSDAM – GERMANY; 2.Benjamin Laulier ,SinapTec Ultrasonic Technology, SYNERGIE PARK, 7 avenue Pierre et Marie Curie 59260 LEZENNES - FRANCE
Literature
May JC, Wheeler RM, Grim E; The Gravimetric Method for the Determination of Residual Moisture in Freeze-Dried Biological Products (1989) Cryobiology 26, 277-284
