Determination of ephedrine alkaloid stereoisomers in dietary supplements by capillary electrophoresis

Phinney, Karen W.; Ihara, Toshihide; Sander, Lane C.

doi:10.1016/j.chroma.2005.04.068

Cited by 55 publications

(35 citation statements)

References 19 publications

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“…Twelve representative diabetes-and obesity-treatment drugs that were considered to be the most frequently used adulterants were selected for analysis: six anti-diabetes drugs (phenformin, rosiglitazone, glipizide, glimepiride, glybenclamide and gliclazide) and six anti-obesity drugs (ephedrine, T3, T4, fenfluramine, fluoxetine and sibutramine; Fig. 1; Cianchino et al, 2008;Julia et al, 2006;Marchei et al, 2006;Phinney et al, 2005;Wang et al, 2008). Other similar obesity-treatment drugs including orlistat and rimonabant were excluded from this study due to rare reports from the market.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of anti‐diabetes/anti‐obesity drugs by LC/PDA, and targeted analysis of sibutramine analog in dietary supplements by LC/MS/MS

Kim

Lee

Yoon

et al. 2009

Biomedical Chromatography

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The safety of dietary supplements is questionable as there have been occasional reports of products contaminated with illegal adulterants. The present study was carried out to develop trustworthy methodologies to screen for six antidiabetic drugs (phenformin, rosiglitazone, glipizide, glimepiride, glybenclamide and gliclazide) and six anti-obesity drugs (ephedrine, fenfluramine, T3, T4, fluoxetine and sibutramine) in dietary supplements. A simultaneous determination method of the 12 drugs by liquid chromatography coupled with a photodiode array (LC/PDA) was established and was validated for linearity (r 2 > 0.99), precision (RSD < < < <13.3%), recoveries (88.8-115.9%) and reproducibility. Sibutramine and its analogs, N-desmethylsibutramine, were subject to further investigation by LC/MS/MS because they were one of the major illegal adulterants. Our proposed method to monitor illegal drug adulterations in dietary supplements using LC/PDA is a simple and reliable, and therefore applicable to routine drug-adulteration screening.

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Section: Introductionmentioning

confidence: 99%

Simultaneous determination of anti‐diabetes/anti‐obesity drugs by LC/PDA, and targeted analysis of sibutramine analog in dietary supplements by LC/MS/MS

Kim

Lee

Yoon

et al. 2009

Biomedical Chromatography

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“…Ephedrine and pseudoephedrine were separated effectively with each other and with the other compounds in the sample in 4 min. Compared with some of the reported methods [4][5][6][7][8][9][10][11][12][13][14][15], the CZE method presented in this paper is simpler, rapid, and possesses higher sensitivity and efficiency.…”

Section: Introductionmentioning

confidence: 94%

“…However, these methods require a derivatization step or exotic mobile phase to allow for separation of the diastereoisomeric substances. In addition, some methods of CE such as nonaqueous CE (NACE) [8], micellar EKC (MEKC) [9], and CZE modified by CD and its derivations [10][11][12][13][14][15] have also been reported. The separation time of these CE methods [8][9][10][11][12][13][14][15] are almost longer than 10 min, and the reproducibility of NACE [8] is not always sufficient.…”

Section: Introductionmentioning

confidence: 99%

Separation and determination of ephedrine and pseudoephedrine in Ephedrae Herba by CZE modified with a Cu(II)–L‐lysine complex

Ding

Cao

2008

Electrophoresis

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A CZE method using a complex of 2.5 mM Cu(II)-L-lysine (molar ratio is 1:2) as additive in a run buffer solution composed of Tris-H(3)PO(4) (pH 4.5) was developed for the simultaneous determination of ephedrine and pseudoephedrine within 4 min. The effects of pH, composition, and concentration of run buffer as well as the composition and concentration of the Cu(II)-L-lysine complex on the separation were investigated. The linear ranges for the determination of ephedrine and pseudoephedrine were 15.0-225.0 and 20.0-250.0 mg/L with LODs both of 5.0 mg/L. Satisfactory result for the determination of ephedrine and pseudoephedrine in Ephedrae Herba from different producing area was obtained by the proposed method. Ephedrine and pseudoephedrine were separated effectively with each other and with the other compounds in the sample. The RSD for the determination of the two constituents in the samples varied from 1.82 to 2.76%, and the recovery ranged between 95.0 and 104.0%.

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“…Binary chiral selectors have been explored for not a short time and have been shown to significantly enhance the enantioresolution of various chiral compounds [11][12][13], including DL-AA derivatized with 5-dimethylamino-naphthalene-1-sulfonyl chloride (combination of b-CD and g-CD) [14], cationic drugs [15] and ephedrine [16] (combination of neutral and anionic CD), 1,1'-binaphthyl-2,2'-diyl hydrogen phosphate (combination of carboxymethylb-CD and sulfobutyl ether-b-CD) [17], some nonsteroidal anti-inflammatory drugs (combination of cationic and anionic CD) [18], and hydrobenzoin (combination of single isomer heptakis(2,3-dihydroxy-6-O-sulfo)-b-CD and b-CD) [19]. Using together a CD and a chiral surfactant has also been shown to be an effective way, which was clearly illustrated in our previous work [10] (see also [20,21] for reviews on CD/bile salt systems).…”

Section: Introductionmentioning

confidence: 99%

Chiral capillary electrophoretic separation of amino acids derivatized with 9‐fluorenylmethylchloroformate using mixed chiral selectors of β‐cyclodextrin and sodium taurodeoxycholate

Chen¹,

Zhang²,

Li³

et al. 2006

Electrophoresis

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Chiral separation of 19 pairs of amino acid (AA) enantiomers derivatized with 9-fluorenylmethylchloroformate (FMOC) was successfully conducted by capillary electrophoresis using the mixture of beta-CD and sodium taurodeoxycholate (STDC) as selectors. Resolution was considerably superior to that obtained by using either beta-CD or STDC alone. After a systematic inspection, a buffer composed of 150 mM borate and 18% v/v isopropanol at pH 8.0, dissolved with 30 mM beta-CD and 30 mM STDC, was adopted and able to generate baseline resolution (>1.50) for 17 pairs of FMOC-AA enantiomers and somewhat lower resolution for arginine (1.36) and alanine (1.18), respectively. Experimental data revealed that the addition of the second selector did not increase the mobility difference between a pair of enantiomers (Delta mu = mu(D) - mu(L) and the number of theoretical plates (N), but decreased the summed apparent mobility of a pair of enantiomers (Sigma mu = mu(D) - mu(L)), which was mainly due to the decrease of the electroosmotic flow. The variation of Sigma mu was thus the major reason responsible for the improvement of chiral resolution in this study. The result demonstrated that not only the intrinsic selectivity of the selectors was the basis of the chiral separation, but also the non-chiral effect of the selectors, the change of the electroosmotic flow, was an important factor in enhancing the enantioseparation resolution. This study could probably help to explain the reasons for resolution improvement in some dual selectors systems, which are not very clear at present.

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Determination of ephedrine alkaloid stereoisomers in dietary supplements by capillary electrophoresis

Cited by 55 publications

References 19 publications

Simultaneous determination of anti‐diabetes/anti‐obesity drugs by LC/PDA, and targeted analysis of sibutramine analog in dietary supplements by LC/MS/MS

Simultaneous determination of anti‐diabetes/anti‐obesity drugs by LC/PDA, and targeted analysis of sibutramine analog in dietary supplements by LC/MS/MS

Separation and determination of ephedrine and pseudoephedrine in Ephedrae Herba by CZE modified with a Cu(II)–L‐lysine complex

Chiral capillary electrophoretic separation of amino acids derivatized with 9‐fluorenylmethylchloroformate using mixed chiral selectors of β‐cyclodextrin and sodium taurodeoxycholate

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