Multi-analysis determination of tropane alkaloids in cereals and solanaceaes seeds by liquid chromatography coupled to single stage Exactive-Orbitrap

Marín-Sáez, Jesús; Romero‐González, Roberto; Frenich, Antonia Garrido

doi:10.1016/j.chroma.2017.08.052

Cited by 38 publications

(40 citation statements)

References 33 publications

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“…The flask was filled with a mixture of methanol: water 2:1 ( v /v), containing 1% acetic acid, and passed through the SPE cartridge. Strata X‐C cartridges were used for the SPE, according to a method previously developed . Briefly, 250 mL of the dissolved sample was passed through the cartridge previously conditioned with 6 mL of methanol and 6 mL of methanol: water 2:1 ( v /v) containing 1% acetic acid.…”

Section: Methodsmentioning

confidence: 99%

“…For the extraction of tropane alkaloids from these types of drugs, only a dilution or dissolution of the samples is needed because of the nature of the matrix. However, since the concentration of tropane alkaloids in homeopathic products is very low, a preconcentration method is needed and for that purpose, a strong cation exchange cartridge can be used …”

Section: Introductionmentioning

confidence: 99%

“…Due to the lack of studies focused on the determination of tropane alkaloids in drugs and homeopathic products, as well as the recent cases and controversy about the homeopathic products containing Belladonna extracts, the aim of this study is the application of a recently developed methodology to search targeted and untargeted tropane alkaloids and other main compounds in homeopathic and Solanaceae‐based drugs, as well as the analysis of Atropa belladonna seeds, which are used for the preparation of these drugs. A simple strong cation exchange solid‐phase extraction (SPE) preconcentration procedure has been performed and ultra‐high performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC–Orbitrap–MS) was used for a reliable identification of the detected compounds.…”

Section: Introductionmentioning

confidence: 99%

“…However, since the concentration of tropane alkaloids in homeopathic products is very low, a preconcentration method is needed and for that purpose, a strong cation exchange cartridge can be used. 29 Due to the lack of studies focused on the determination of tropane alkaloids in drugs and homeopathic products, as well as the recent cases and controversy about the homeopathic products containing Belladonna extracts, the aim of this study is the application of a recently developed methodology 29 to search targeted and untargeted tropane alkaloids and other main compounds in homeopathic and Solanaceae-based drugs, as well as the analysis of Atropa belladonna seeds, which are used for the preparation of these drugs.…”

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confidence: 99%

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Screening of drugs and homeopathic products from Atropa belladonna seed extracts: Tropane alkaloids determination and untargeted analysis

Marín-Sáez

Romero-González

Frenich

et al. 2018

Drug Testing and Analysis

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Homeopathic products are still a controversial issue in modern medicine, understood as complementary or alternative medicine (CAM). In this particular case, homeopathic products prepared from Atropa belladonna extracts may present specific problems due to the effects derived from its components. This article applies a simple, rapid, reliable method to the analysis of different homeopathic products obtained from Atropa belladonna; drugs containing high concentration of plant extracts; and Atropa belladonna seeds. The method was based on a simple solid-phase preconcentration method followed by ultra-high pressure liquid chromatography (UHPLC) coupled to high resolution mass spectrometry using Exactive-Orbitrap as an analyser. An in-house database was set and atropine and scopolamine were the compounds detected at highest concentrations in homeopathic products from Atropa belladonna extracts (4.57 and 2.56 μg/kg, respectively), in Belladonna ointment (4007 and 1139 μg/kg, respectively) and Belladonna seeds (338 and 32.1 mg/kg, respectively). Other tropane alkaloids such as tropine, apoatropine, aposcopolamine, tropinone, homatropine, and anisodamine were detected at lower concentrations (0.04-1.36 μg/kg). When untargeted analysis was performed, other tropane alkaloids were identified in the tested samples, such as ecgonine (0.003 μg/kg), benzoylecgonine (0.56 μg/kg), calystegines A (19.6 μg/kg), B (33.1 μg/kg), and C (1.01 μg/kg). Finally other compounds present in the homeopathic products, such as sugars (fructose, glucose, and lactose) or amino acids (valine, ornithine, leucine, and phenylalanine), were identified.

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

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Screening of drugs and homeopathic products from Atropa belladonna seed extracts: Tropane alkaloids determination and untargeted analysis

Marín-Sáez

Romero-González

Frenich

et al. 2018

Drug Testing and Analysis

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“…Tropane alkaloids occur naturally in many members of the plant family Solanaceae. Total synthesis for tropane alkaloids is an efficient way to obtain those active compounds since their content in natural products is very low [11]. Total synthesis for tropane alkaloids is an efficient way to obtain those active compounds since their content in natural products is very low [11].…”

Section: Introductionmentioning

confidence: 99%

Enantioseparation of acetyltropic acid by countercurrent chromatography with sulfobutyl ether‐β‐cyclodextrin as chiral selector

Qiu

Sun

Wang

et al. 2019

J of Separation Science

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Acetyltropic acid is an important synthetic intermediate for preparation of tropane alkaloid derivatives, which can be used as anticholinergic drugs, deliriants, and stimulants. In the present work, acetyltropic acid was successfully enantioseparated by countercurrent chromatography using sulfobutyl ether-β-cyclodextrin as chiral selector. A biphasic solvent system composed of n-butyl acetate/n-hexane/0.1 mol/L citrate buffer at pH = 2.2 containing 0.1 mol/L of sulfobutyl ether-β-cyclodextrin (7:3:10, v/v) was selected, which produced a suitable distribution ratio D S = 1.14, D R = 2.31 and a high enantioseparation factor α = 2.03. Baseline separation was achieved for preparative enantioseparation of 50 mg of racemic acetyltropic acid. A method for chiral analysis of acetyltropic acid by conventional reverse phase liquid chromatography with hydroxylpropyl-β-cyclodextrin as mobile phase additive was established, and formation constants of inclusion complex were determined. It was found that different substituted β-cyclodextrin should be selected for enantioseparation of acetyltropic acid by countercurrent chromatography and reverse phase liquid chromatography. K E Y W O R D Sacetyltropic acid, countercurrent chromatography, cyclodextrins, enantioseparation, liquid chromatography J Sep Sci 2020;43:681-688.

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Occurrence and Determination of Tropane Alkaloids in Food and Feed

Gonçalves

Dernovics

Moreno‐González

et al. 2020

Encyclopedia of Analytical Chemistry

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The determination of tropane alkaloids (TAs) in food and feed is gaining importance after the detection of mainly atropine and scopolamine in cereal and tea/herbal infusion samples at levels that may represent a risk to human health, in particular for infants and young children. Relevant legislation was published in the European Union (EU) recently. This article aims at presenting the most recent developments in the sample preparation and analytical determination of this group of substances in food and feed. Considerations about related matrices are also included with the purpose of gaining insight into other alternative and advanced analytical approaches. A review of the occurrence and levels of TAs in food and feed until 2019 covering EU‐wide surveys, data archived in the official notifications repository and the scientific literature is carried out as well, since such data are needed for any risk assessment.

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Multi-analysis determination of tropane alkaloids in cereals and solanaceaes seeds by liquid chromatography coupled to single stage Exactive-Orbitrap

Cited by 38 publications

References 33 publications

Screening of drugs and homeopathic products from Atropa belladonna seed extracts: Tropane alkaloids determination and untargeted analysis

Screening of drugs and homeopathic products from Atropa belladonna seed extracts: Tropane alkaloids determination and untargeted analysis

Enantioseparation of acetyltropic acid by countercurrent chromatography with sulfobutyl ether‐β‐cyclodextrin as chiral selector

Occurrence and Determination of Tropane Alkaloids in Food and Feed

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