Identification of steroid drugs by13C NMR spectroscopy

Kartashov, V. S.; Shorshnev, S. V.; Арзамасцев, А. П.

doi:10.1007/bf00777149

Cited by 2 publications

(2 citation statements)

References 13 publications

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“…These data can be used for identification of the drugs. Previously [2] we have identified the above compounds by the ~H NMR technique. However, the t3C NMR spectra are more convenient for identification purposes than the 1H NMR spectra comprising involved multilplets of proton signals.…”

Section: Identification Of Drugs Belonging To the Anilide Series By 1mentioning

confidence: 99%

Identification of drugs belonging to the anilide series by13C NMR spectroscopy

Kartashov

1999

Pharm Chem J

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Section: Identification Of Drugs Belonging To the Anilide Series By 1mentioning

confidence: 99%

Identification of drugs belonging to the anilide series by13C NMR spectroscopy

Kartashov

1999

Pharm Chem J

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“…Therefore it is necessary to ®nd a sensitive analytical method for the determination of PRO. Several methods have been developed to determine PRO including high performance liquid chromatography (HPLC) [2±5], capillary electrophoresis (CE) [6±9], micellar electrokinetic capillary chromatography (MEKC) [10], gas chromatography (GC) [11,12], gel chromatography [13], thin layer chromatography (TLC) [14], nuclear magnetic resonance (NMR) [15], spectrophotometry [16] and¯uorescence spectrometry [17,18]. And the detection modes in these references are usually UV=vis absorbance [2±4, 7±8],¯uorescence spectrometry [6], mass spectrometry (MS) [9,11] and photodiode array detector [5].…”

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Determination of Propranolol by Capillary Electrophoresis with End-Column Amperometric Detection

et al. 2000

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A capillary electrophoresis-amperometric detection system was developed for the determination of propranolol (PRO) at a 33 mm carbon ®ber microdisk electrode (CFE). The cyclic voltammogram, the hydrodynamic voltammograms and the effect of pH were studied. Under the optimum conditions: separation voltage 15 kV; injection 3 s at 15 kV; 10 mM pH 7.5 phosphate buffer, 1.15 V (vs. Ag=AgCl) detection potential, the detection limit (LOD) for PRO was 0.05 mM (S=N 3). The response for PRO was linear over two orders of magnitude with a linear correlation coef®cient of 0.994. The feasibility of this method was demonstrated by the detection of PRO in urine sample.Keywords: Capillary electrophoresis, End-column amperometic detection, Propranolol Propranolol (PRO) is a b-adrenergic blocking agent (pK a 9.45 [1]). The structure of PRO is given in Figure 1. It is used in the treatment of hypertension and cardiovascular disorder. But bblockers are exceptionally toxic and most of them possess a narrow therapeutic range, the difference between the lowest therapeutic and highest tolerable doses is small. Therefore it is necessary to ®nd a sensitive analytical method for the determination of PRO. Several methods have been developed to determine PRO including high performance liquid chromatography (HPLC) [17,18]. And the detection modes in these references are usually UV=vis absorbance [2±4, 7±8],¯uorescence spectrometry [6], mass spectrometry (MS) [9,11] and photodiode array detector [5]. So far no report about electrochemical detection (EC) of PRO in CE has been published. CE-EC possesses many advantages including lower injection volume and consumption of solvent, high sensitivity, selectivity comparing to other methods. In the present article, the amperometric detection (AD) method for the determination of PRO separated by capillary zone electrophoresis (CZE) was reported. The end-column AD mode is simple and sensitive. Without any modi®cation and sample concentration, the LOD of this method is several decades lower than UV detector reported [11].Before each run, the capillary is¯ushed consequently with doubly distilled water, NaOH (0.1 M), doubly distilled water and buffer for 1, 1, 1, 5 min, respectively. The proper alignment of the microelectrode with the bore of the capillary is achieved by microscope. The distance between the electrode and the end of the capillary is about 30 mm to get high signal-to-noise ratio and good reproducibility. The preparation of the CFE is same as [19]. Before use in the detection of CE, the microelectrode is polished with different kinds of Al 2 O 3 powder, washed with doubly distilled water, sonicated by an ultrasonic wave cleaner, respectively. During the experiment, the electrode tends to be poisoned and the peak currents decrease gradually without any treatment on the electrode. We found that electrochemical treatment can activate the surface of the electrode and hence improve the reproducibility. The CFE is swept 50 mV=s between À0.3 V±1.4 V (vs. Ag=AgCl) for 2 min in order to clean...

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Identification of steroid drugs by13C NMR spectroscopy

Cited by 2 publications

References 13 publications

Identification of drugs belonging to the anilide series by13C NMR spectroscopy

Identification of drugs belonging to the anilide series by13C NMR spectroscopy

Determination of Propranolol by Capillary Electrophoresis with End-Column Amperometric Detection

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