Sensitive ergotamine determination in pharmaceuticals and biological samples using cloud point preconcentration and spectrofluorimetric detection

Wang, Chien-Chun; Fernández, Liliana Patricia; Gómez, María R.

doi:10.1016/j.aca.2013.01.023

Cited by 12 publications

(5 citation statements)

References 22 publications

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“…Nonionic surfactant PONPE 7.5 (Fig. ) was selected for CPE because of some experimental advantage such as low critical cloud point and low UV‐Visible signal background . In order to study the influence of experimental parameters on CPE, a systematic study was applied for each parameter.…”

Section: Resultsmentioning

confidence: 99%

“…In our previous works, CPE has proved to be efficient for monitoring drugs level in biological samples. The most important advantage of CPE is that only a small amount of surfactant is required and consequently the procedure is less expensive and more environmentally friendly than other conventional extraction techniques such as liquid extraction and solid–liquid extraction . Moreover, CPE offers the possibility of combining extraction and preconcentration in one step.…”

Section: Introductionmentioning

confidence: 99%

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Simultaneous separation of ergot alkaloids by capillary electrophoresis after cloud point extraction from cereal samples

et al. 2014

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A new and sensitive analytical methodology for ergot alkaloids (EA) determination from cereal samples based on cloud point extraction (CPE) prior to CE-UV absorbance was developed. The methodology involves extraction under acid conditions and subsequent preconcentration by applying a simple, rapid and environmentally friendly low volume surfactant extraction procedure. After extraction, CE analysis was carried out by performing dilutions on preconcentrated surfactant rich phase, achieving a single peak or simultaneous alkaloids determination. A real preconcentration factor of 22 of total EA was obtained, demonstrating the efficiency of this methodology. The limits of detection were 2.6 and 2.2 μg/kg for ergotamine and ergonovine, respectively. Validation procedure revealed suitable linearity, accuracy and precision. The average extraction and clean-up recoveries were compared with the theoretical values and were better than 92%. This method was successfully applied to the determination of EA in different varieties of commercial flour samples, two grain samples and one of the leading brands cereal-based product for infant feeding. The high sensitivity achieved for EA determinations in real samples suggests CPE procedure as an interesting approach to improve CE-UV visible detection limits. Moreover, the whole process could be considered as a contribution to green chemistry because nonorganic solvents were involved, demonstrating its great potential over conventional techniques.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Simultaneous separation of ergot alkaloids by capillary electrophoresis after cloud point extraction from cereal samples

et al. 2014

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“…The ELISA method has been used primarily when scientists are interested in determining the concentration of total ergot alkaloids, not particular alkaloids (Stuedemann et al, 1998; Hill et al, 2000; Ayers et al, 2009). However, the ELISA assay lacks selectivity as it does not differentiate between ergot alkaloids which have necessitated the use of chromatographic methods to detect specific ergot alkaloids (Schultz et al, 2006; De Lorme et al, 2007; Foote et al, 2012; Wang et al, 2013). Schnitzius et al (2001), compared HPLC and ELISA detection of ergot alkaloids and found the methods were inconsistent in their identification of alkaloids, concluding that both had their advantages and disadvantages.…”

Section: Discussionmentioning

confidence: 99%

“…Initially, chromatographic methods had relatively high detection limits (Yates and Powell, 1988; Rottinghaus et al, 1991; Moubarak et al, 1996); however, more recent advances in chromatographic and detection methods have vastly improved the sensitivities of the assays (Lehner et al, 2005; Smith et al, 2009; Foote et al, 2012; Wang et al, 2013). Enzyme linked immunosorbent assay is a faster method for detection of ergot alkaloids and has been used to screen livestock exposure to fescue toxins (Shelby and Kelley, 1990; Hill and Agee, 1994).…”

Section: Introductionmentioning

confidence: 99%

Relationships among ergot alkaloids, cytochrome P450 activity, and beef steer growth

Rosenkrans

Ezell

2015

Front. Chem.

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Determining a grazing animal's susceptibility to ergot alkaloids has been a research topic for decades. Our objective was to determine if the Promega™ P450-Glo assay could be used to indirectly detect ergot alkaloids or their metabolites in urine of steers. The first experiment validated the effects of ergot alkaloids [0, 20, and 40 μM of ergotamine (ET), dihydroergotamine (DHET), and ergonovine (EN)] on human CYP3A4 using the P450-Glo assay (Promega™ V9800). With this assay, luminescence is directly proportional to CYP450 activity. Relative inhibition of in vitro cytochrome P450 activity was affected (P < 0.001) by an interaction between alkaloids and concentration. That interaction resulted in no concentration effect of EN, but within ET and DHET 20 and 40 μM concentrations inhibited CYP450 activity when compared with controls. In experiment 2, urine was collected from Angus-sired crossbred steers (n = 39; 216 ± 2.6 days of age; 203 ± 1.7 kg) after grazing tall fescue pastures for 105 days. Non-diluted urine was added to the Promega™ P450-Glo assay, and observed inhibition (3.7 % ± 2.7 of control). Urine content of total ergot alkaloids (331.1 ng/mg of creatinine ± 325.7) was determined using enzyme linked immunosorbent assay. Urine inhibition of CYP450 activity and total alkaloids were correlated (r = −0.31; P < 0.05). Steers were genotyped at CYP450 single nucleotide polymorphism, C994G. Steer genotype affected (P < 0.03) inhibition of CYP450 activity by urine; heterozygous steers had the least amount of CYP450 inhibition suggesting that genotyping cattle may be a method of identifying animals that are susceptible to ergot alkaloids. Although, additional research is needed, we demonstrate that the Promega™ P450-Glo assay is sensitive to ergot alkaloids and urine from steers grazing tall fescue. With some refinement the P450-Glo assay has potential as a tool for screening cattle for their exposure to fescue toxins.

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“…EGT in urine, blood, and hair samples has also been identified using an LC-MS method [ 17 ]. A spectrofluorimetry technique was also used to measure EGT in pharmaceuticals, urine, and saliva samples [ 18 ]. EGT, caffeine, and metamizol are all simultaneously determined using a high-performance thin-layer chromatography (HPTLC) method from combined dosage form [ 19 ].…”

Section: Introductionmentioning

confidence: 99%

A Rapid and Sensitive Stability-Indicating Eco-Friendly HPTLC Assay for Fluorescence Detection of Ergotamine

et al. 2023

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Eco-friendly liquid chromatographic methods for measuring ergotamine (EGT) are scant in the published database. Accordingly, the goal of the current study was to develop a high-performance thin-layer chromatography (HPTLC) method for fluorescence detection of EGT in commercially available tablets. This approach was based on the application of ethyl alcohol–water (80:20 v/v) as the eco-friendly eluent mixture. The fluorescence detection of EGT was carried out at 322 nm. The greenness score of the present approach was evaluated by “Analytical GREENness (AGREE)” technology. The present approach for measuring EGT in the 25–1000 ng band−1 range was linear. The present assay for fluorescence detection of EGT was validated successfully by ICH guidelines for various parameters. The method was found to be rapid, sensitive, eco-friendly, and stability-indicating. The computed AGREE index for the current strategy was 0.84, displaying outstanding greenness features. The present methodology successfully separated the EGT degradation products under forced-degradation circumstances, exhibiting its stability-indicating qualities and selectivity. An amount of 99.33% of EGT was found in commercial formulations, indicating the validity of the current method for pharmaceutical analysis of EGT in commercial products. The results showed that EGT in commercial products might be regularly measured by the existing method.

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Sensitive ergotamine determination in pharmaceuticals and biological samples using cloud point preconcentration and spectrofluorimetric detection

Cited by 12 publications

References 22 publications

Simultaneous separation of ergot alkaloids by capillary electrophoresis after cloud point extraction from cereal samples

Simultaneous separation of ergot alkaloids by capillary electrophoresis after cloud point extraction from cereal samples

Relationships among ergot alkaloids, cytochrome P450 activity, and beef steer growth

A Rapid and Sensitive Stability-Indicating Eco-Friendly HPTLC Assay for Fluorescence Detection of Ergotamine

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