Wyniki wyszukiwania - BazTech

1

Multiphase extraction of ephedrine from Pinellia ternata using bionic liquid-modified polymer

Fang Luwei, Tian Minglei, Lin Liangwen, Row Kyung Ho

Polish Journal of Chemical Technology

|

2019

|

Vol. 21, nr 4

13--19

EN

Multiphase extraction (MPE) was applied as a developed, convenient and efficient method in separation of ephedrine from Pinellia ternata. Firstly, in order to increase the adsorption efficiency, bionic liquid-modified polymer was created. Comparing the effects of all sorbents under variables conditions, the highest amount of 5.8 mg/g can be adsorbed on dual imidazole ionic liquid modified polymer (Im-Im-Poly) in methanol/water (70:30, v/v) solution at 25°C within 30.0 min. Then the Im-Im-Poly was applied in MPE, after 7 times repetition of extraction, around 1.0 mg/g of ephedrine from Pinellia ternata was detected. After washing by water, ethanol and methanol, and elution by methanol/acetic acid (99.0:1.0, v/v), ephedrine was successfully separated.

2

Development micellar HPLC method for simultaneous determination of ephedrine, pseudoephedrine, and methylephedrine in Ephedra Herb and traditional Chinese medicinal preparations

Dong Y. M., An Q., Lu N. W., Li N.

Acta Chromatographica

|

2015

|

Vol. 27, no. 2

355--372

EN

A micellar high-performance liquid chromatography (HPLC) method has been described for simultaneous determination of ephedrine, pseudoephedrine, and methylephedrine in Ephedra Herb and two traditional Chinese preparations. The separation and determination of ephedrine, pseudoephedrine, and methylephedrine were performed using a mobile phase containing 1.75 × 10−1 mol•L−1 sodium dodecyl sulphate and 0.02 mol•L−1 potassium hydrogen phosphate with 10% (v/v) methanol at pH 3.0, running at 1.5 mL•min−1 by a Venusil XBP C18 (250 × 4.6 mm, 5 μm) column at 40 °C. The detected wavelength was set at 210 nm. The method was validated according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) guidelines. The main analytical parameters were linearity (r > 0.9990), intra- and inter-day precisions (relative standard deviation [RSD %], 0.33–1.63, and RSD %, 1.26–2.20, respectively), limit of quantifications [LOQs], and limit of detections [LODs] (2.6 × 10−4 and 7.8 × 10−5 mg•mL−1 for ephedrine, 6.8 × 10−4 and 2.0 × 10−4 mg•mL−1 for pseudoephedrine, and 5.0 × 10−4 and 1.5 × 10−4 mg•mL−1 for methylephedrine). RSDs of recoveries were <5.5% in the three samples. Based on the optimized chromatographic conditions and the eluted orders, a model of separation mechanism for the analytes was established. The results indicated that the proposed method was an accurate, “green” and cheap method.

3

Simultaneous RP-IP-HPLC assay of theophylline, phenobarbital, codeine, and ephedrine in a suppository

Jankovics P, Németh T, Németh-Palotás J, Kőszegi-Szalai H

Acta Chromatographica

|

2010

|

Vol. 22, no. 4

527--538

EN

A reversed-phase ion-pairing liquid chromatographic (RP-IP-HPLC) method for simultaneous assay of theophylline (TH), phenobarbital (PB), codeine (CD), and ephedrine (EP) in an extemporaneous (magistral) suppository was developed and validated and used to investigate a reported serious adverse event. Samples were dissolved in dichloromethane and extracted by two-step liquid-liquid extraction with acetate buffer (pH 5.0) and, subsequently, 0.1 M NaOH solution. Separation was performed on an end-capped C 18 silica column with stepwise gradient elution. Sample preparation and chromatographic conditions were optimized on the basis of the p K a values of the analytes. Freedom from interference from the excipients, linearity ( r 2 > 0.999 for all the active ingredients), range (0.01–0.08 mg mL -1 for TH, CD, and EP; 0.0025–0.02 mg mL -1 for PB), intra-day and inter-day precision, and accuracy (recovery >95% for TH, CD, and EP and >90% for PB) of the method were demonstrated. Non-compliance of the examined product was confirmed.