Optimized Analysis of Ergot Alkaloids in Rye Products by Liquid Chromatography-Fluorescence Detection Applying Lysergic Acid Diethylamide as an Internal Standard

Analysis of ergot alkaloids remains a topic of importance and the European Food Safety Authority (EFSA) has encouraged laboratories to provide monitoring data for the further evaluation of their occurrence in food and feed. While LC-MS/MS has dominated developments in recent years, LC-FLD is still more widespread, especially in developing countries. To improve the analysis of ergot alkaloids by LC-FLD, we developed an improved protocol introducing lysergic acid diethylamide (LSD) for internal standardization. Several aspects such as the composition and pH of the extraction medium, type of sorbent and conditions applied for solid-phase extraction/clean-up, use of a keeper during final evaporation and the type of syringe filter used for filtration prior to injection were thoroughly investigated. Optimized conditions comprise extraction by ethyl acetate, methanol and 28% aqueous ammonia in combination with basic aluminum oxide for extract clean-up. Use of a keeper was found inappropriate as LC-FLD analysis was significantly affected by co-eluting keeper components. Similar observations were made with some of the investigated syringe filters, where polytetrafluoroethylene (PTFE) proved to be the most suitable. Validation and application of the optimized methodology to real samples provided limits of detection and quantification suitable for the evaluation of relevant ergot alkaloid contaminations in rye and bakery products with superior precision that was facilitated by the introduced internal standard, LSD.

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Validation of a New Sensitive Method for the Detection and Quantification of R and S-Epimers of Ergot Alkaloids in Canadian Spring Wheat Utilizing Deuterated Lysergic Acid Diethylamide as an Internal Standard

Toxins ◽

10.3390/toxins14010022 ◽

2021 ◽

Vol 14 (1) ◽

pp. 22

Author(s):

Jensen Cherewyk ◽

Taylor Grusie-Ogilvie ◽

Barry Blakley ◽

Ahmad Al-Dissi

Keyword(s):

Spring Wheat ◽

Matrix Effects ◽

Limit Of Detection ◽

Ergot Alkaloids ◽

Internal Standard ◽

Lysergic Acid ◽

Lysergic Acid Diethylamide ◽

Relative Standard ◽

Validation Parameters ◽

Sensitive Method

Ergot sclerotia effect cereal crops intended for consumption. Ergot alkaloids within ergot sclerotia are assessed to ensure contamination is below safety standards established for human and animal health. Ergot alkaloids exist in two configurations, the R and S-epimers. It is important to quantify both configurations. The objective of this study was to validate a new ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for quantification of six R and six S-epimers of ergot alkaloids in hard red spring wheat utilizing deuterated lysergic acid diethylamide (LSD-D3) as an internal standard. Validation parameters such as linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effects, recovery and precision were investigated. For the 12 epimers analyzed, low LOD and LOQ values were observed, allowing for the sensitive detection of ergot epimers. Matrix effects ranged between 101–113% in a representative wheat matrix. Recovery was 68.3–119.1% with an inter-day precision of <24% relative standard deviation (RSD). The validation parameters conform with previous studies and exhibit differences between the R and S-epimers which has been rarely documented. This new sensitive method allows for the use of a new internal standard and can be incorporated and applied to research or diagnostic laboratories.

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Physiological Effects of Schizophrenic Body Fluids

Journal of Mental Science ◽

10.1192/bjp.105.438.1 ◽

1959 ◽

Vol 105 (438) ◽

pp. 1-18 ◽

Cited By ~ 9

Author(s):

Edith G. McGeer ◽

Patrick L. McGeer

Keyword(s):

Ergot Alkaloids ◽

Body Fluids ◽

Lysergic Acid ◽

Mental Illnesses ◽

Lysergic Acid Diethylamide ◽

Organic Basis ◽

Physiological Effects ◽

Chemical Agents ◽

Mental Disturbances

Controversy has raged for over half a century as to whether schizophrenia, the most severe of all mental illnesses, could have an organic basis or whether its origin lay strictly in the psyche. Over the years, physiologists have probed into almost every aspect of the soma in the quest for some abnormality which would account for the schizophrenic syndrome. Many possibilities have been considered, investigated to a degree and then abandoned when definitive answers were not forthcoming. A dominant approach throughout has been the search for some psychotoxic material circulating in schizophrenic body fluids. Activity has been spurred by the recurrent recognition that chemical agents such as the ergot alkaloids, mescaline, bulbocapnine and lysergic acid diethylamide (LSD-25), could induce in normal persons transient mental disturbances similar to those seen in schizophrenia.

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DEVELOPMENT OF A TECHNIQUE FOR THE MASS-SPECTROMETRIC DETERMINATION OF GONADOTROPIN-RELEASING HORMONE AND ITS ANALOGS FOR DOPING CONTROL

Тонкие химические технологии ◽

10.32362/2410-6593-2017-12-2-81-99 ◽

2017 ◽

Vol 12 (2) ◽

pp. 81-99

Author(s):

K. M. Shestakova ◽

G. A. Dudko ◽

M. A. Dikunets

Keyword(s):

Matrix Effects ◽

Limit Of Detection ◽

Solid Phase ◽

Internal Standard ◽

Ion Source ◽

Gonadotropin Releasing Hormone ◽

Selected Reaction Monitoring ◽

Releasing Hormone ◽

Optimized Conditions

In the present study, a rapid, sensitive, and selective method for determination of several synthetic analogues of gonadotropin-releasing hormone in human urine by solid-phase extraction and ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was developed. Various parameters affecting sample preparation, LC separation, and MS/MS detection were investigated, and optimized conditions were identified. The UPLC-MS/MS system was equipped with an electrospray ion source operating in positive ion mode with selected reaction monitoring. Leuprolide-13С6 was used as internal standard for analytes quantitative assessment. The proposed method was validated considering the parameters specificity, linearity (0.1-10 ng/ml), recovery (52-98%), limit of detection (0.1 ng/ml), matrix effects and stability.

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Cleaving Ergot Alkaloids by Hydrazinolysis—A Promising Approach for a Sum Parameter Screening Method

Toxins ◽

10.3390/toxins13050342 ◽

2021 ◽

Vol 13 (5) ◽

pp. 342

Author(s):

Maximilian Kuner ◽

Susanne Kühn ◽

Hajo Haase ◽

Klas Meyer ◽

Matthias Koch

Keyword(s):

Acid Derivative ◽

Ergot Alkaloid ◽

Reaction Rate ◽

Model Compound ◽

Screening Method ◽

Ergot Alkaloids ◽

Reaction Times ◽

Lysergic Acid ◽

Ammonium Iodide ◽

Food And Feed

Ergot alkaloids are mycotoxins formed by fungi of the Claviceps genus, which are some of the most common contaminants of food and feed worldwide. These toxins are a structurally heterogeneous group of compounds, sharing an ergoline backbone. Six structures and their corresponding stereoisomers are typically quantified by either HPLC-FLD or HPLC-MS/MS and the values subsequently summed up to determine the total ergot alkaloid content. For the development of a screening method targeting all ergot alkaloids simultaneously, the alkaloids need to be transferred to one homogeneous structure: a lysergic acid derivative. In this study, two promising cleaving methods—acidic esterification and hydrazinolysis—are compared, using dihydroergocristine as a model compound. While the acidic esterification proved to be unsuitable, due to long reaction times and oxidation sensitivity, hydrazinolysis reached a quantitative yield in 40‒60 min. Parallel workup of several samples is possible. An increasing effect on the reaction rate by the addition of ammonium iodide was demonstrated. Application of hydrazinolysis to a major ergot alkaloid mix solution showed that all ergopeptines were cleaved, but ergometrine/-inine was barely affected. Still, hydrazinolysis is a suitable tool for the development of a sum parameter screening method for ergot alkaloids in food and feed.

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The Therapeutic Value of Lysergic Acid Diethylamide in Mental Illness

Journal of Mental Science ◽

10.1192/bjp.100.419.491 ◽

1954 ◽

Vol 100 (419) ◽

pp. 491-507 ◽

Cited By ~ 88

Author(s):

R. A. Sandison ◽

A. M. Spencer ◽

J. D. A. Whitelaw

Keyword(s):

Mental Illness ◽

Secondary Amine ◽

Ergot Alkaloids ◽

Lysergic Acid ◽

Mental Illnesses ◽

Lysergic Acid Diethylamide ◽

Repressed Memories ◽

Therapeutic Value ◽

The Subject ◽

One Year

D-lysergic acid diethylamide (LSD 25) was first prepared in 1938 by Stoll and Hofmann. It is the synthetic amide of d-lysergic acid with a secondary amine, diethylamine and belongs to the ergonovine group of ergot alkaloids all of which have lysergic acid as a base. After its ingestion in minute doses, it induces psychic states in which the subject becomes aware of repressed memories and other unconscious material in a setting of clear consciousness. This preliminary paper describes the results obtained from the use of the drug in 36 psychoneurotic patients over a period of one year. We consider that the drug will find a significant place in the treatment of the psychoneuroses and allied mental illnesses.

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Bioanalytical method development and validation of simultaneous analysis of telmisartan and hydrochlorthiazide in human plasma using LC-MS/MS

International Journal of Bioassays ◽

10.21746/ijbio.2016.03.003 ◽

2016 ◽

Vol 5 (03) ◽

pp. 4862 ◽

Cited By ~ 1

Author(s):

Mathew George* ◽

Lincy Joseph ◽

Arpit Kumar Jain ◽

Anju V.

Keyword(s):

Human Plasma ◽

Retention Time ◽

High Performance ◽

Method Development ◽

Matrix Effects ◽

Solid Phase ◽

Internal Standard ◽

Assay Method ◽

Buffer System ◽

Internal Standards

A simple, sensitive, rapid and economic high performance thin layer chromatographic method and a mass spectroscopic assay method has been developed for the quantification of telmisartan and hydrochlorthiazide combination in human plasma. The internal standards and analytes were extracted from human plasma by solid-phase extraction with HLB Oasis1cc (30mg) catridges. The scanning and optimization for the samples are done using methanol: water (50:50). The samples were chromatographed using reverse phase chromatography with C-18 column of different manufacturers like Ascentis C18 (150×4. 6, 5µ) using the buffer system Acetonitrile: Buffer (80:20%v/v) which consist of 2±0. 1Mm ammonium format at a flow rate of 0. 7ml/min at a column oven temperature 35±10c. The internal standard used was hydrochlorthiazide13c1, d2 and telmisartand3. The extraction techniques include conditioning, loading, washing and elution, drying followed by reconstitution of the dried samples. The volume injected was 10µl with the retention time of 3-4 min for telmisartan, 1-2 min for hydrochlorthiazide and for the internal standards the retention time was 3-4 min for telmisartand3 and 1-2 min for hydrochlorthiazide c13d2. The rinsing solution was Acetonitrile: HPLC grade water in the ratio (50:50). The above developed method was validated using various parameters like selectivity and sensitivity, accuracy and precision, matrix effects, % recovery and various stability studies. The method was proved to be sensitive, accurate, precise and reproducible. The preparation showed high recovery for the quantitative determination of telmisartan and hydrochlorthiazide in human plasma.

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A solid-phase extraction method that eliminates matrix effects of complex pulp mill effluents for the analysis of lipophilic wood extractives

Nordic Pulp & Paper Research Journal ◽

10.1515/npprj-2020-0039 ◽

2020 ◽

Vol 35 (4) ◽

pp. 577-588

Author(s):

Sebastian España Orozco ◽

Philipp Zeitlinger ◽

Karin Fackler ◽

Robert H. Bischof ◽

Antje Potthast

Keyword(s):

Solid Phase Extraction ◽

Matrix Effects ◽

Solid Phase ◽

Internal Standard ◽

Pulp Mill ◽

Phase Extraction ◽

Wood Extractives ◽

Wood Extractive ◽

Pulp Mill Effluents ◽

The Impact

AbstractThe extraction of lipophilic wood extractives from pulp and paper process waters proves to be a challenging task, due to harsh and alternating process and sample conditions. This study has determined the potential use of polymeric sorbents for solid-phase extraction (SPE) and compared to classical silica-based reversed-phase packed columns, with polymeric hydrophilic-lipophilic balanced (HLB) cartridges being the sorbent with the most potential. Recovery functions were obtained with an internal standard mixture representative for the main lipophilic wood extractive groups, which are fatty acids and alcohols, sterols, sterol esters and triglycerides. The impact of pH, sample volume and sample matrix, expressed as TOC and cations, on the retention behavior of lipophilic extractives during SPE of industrial samples were determined with polymeric HLB sorbent. High variations in the composition of pulp mill matrices led to different optimal extraction conditions. Thus, a new SPE protocol was developed, which bypasses matrix interferences and omits the loss of analytes due to sample preparation. The method is applicable to different pulp mill effluents with large discrepancies in pH and sample matrices, resulting in recoveries >90 % with RSD <5 % for all lipophilic wood extractives.

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Changes in Online Psychoactive Substance Trade via Telegram during the COVID-19 Pandemic

European Addiction Research ◽

10.1159/000516853 ◽

2021 ◽

pp. 1-6

Author(s):

Matthijs Blankers ◽

Daan van der Gouwe ◽

Lavinia Stegemann ◽

Laura Smit-Rigter

Keyword(s):

Social Media ◽

The Netherlands ◽

Relative Increase ◽

Lysergic Acid ◽

Lysergic Acid Diethylamide ◽

Psychoactive Substance ◽

Before And After ◽

Other Substances

Background: In this article, we present an evaluation of online psychoactive substance trade via Telegram, a free encrypted social media messenger service. The evaluation took place during the COVID-19 pandemic, which allowed us to monitor the effects of the spring 2020 lockdown in the Netherlands on substance trade via Telegram. Objective: The objective of this study was to evaluate whether changes in psychoactive substance trade on Telegram markets in the Netherlands can be observed during the COVID-19 pandemic. Results: Between December 2, 2019, and June 29, 2020, a total of 70,226 posts appeared in two analyzed Telegram groups. A total of 5,643 posts were psychoactive substance related. Based on the analyzed posts, Telegram is mostly a ‘“sellers” market as only a minority of the posts (6.3%) could be identified as a request for a substance. The proportion of posts related to specific substances varied between the periods before, during, and after the lockdown. The proportion of posts on the stimulants ecstasy, cocaine, and amphetamine was lower during the lockdown than before and after. For psychedelics – ketamine, lysergic acid diethylamide (LSD), and 2,5-dimethoxy-4-bromophenethylamine (2C-B) – and other substances, there was a relative increase in the number of posts during the lockdown, which was maintained after the lockdown. Conclusions: Telegram analysis shows that in the Netherlands, online psychoactive substance trade may have been affected during the COVID-19 pandemic. The direction of this effect was different for different classes of substances.

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