Sinaptec NexTgen 系列設(shè)備成功應(yīng)?于快速制備?基型庫侖滴定法(電量滴定) Ultrasound-assisted rapid preparation of water standards for Karl Fischer coulometric titration

快速量化?基型庫侖滴定法(電量滴定)實(shí)驗(yàn)實(shí)現(xiàn)省時(shí)且可復(fù)制性

利? Sinaptec NexTgen 超聲設(shè)備提供的超聲環(huán)境和相關(guān)溶劑(甲醇和?甲基亞砜) 成功實(shí)現(xiàn)從酒?酸鈉??化合物中提取?,不僅實(shí)現(xiàn)可重復(fù)性和可復(fù)制性,?且實(shí)現(xiàn)快速制備以達(dá)到節(jié)約寶貴時(shí)間?的.

可快速實(shí)現(xiàn)對(duì)藥物,?物等含?量化測(cè)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)

實(shí)驗(yàn)綜合結(jié)論

與傳統(tǒng)樣品制備相?,超聲環(huán)境反應(yīng)下效果明顯,省時(shí)性和低成本性突出. Significant time and cost savings compared to traditional sample preparation workflows based on

應(yīng)?設(shè)備參考

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).

應(yīng)?學(xué)者及?獻(xiàn)來源信息

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