• Analytical Science and Technology
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• v.35 no.2
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• pp.82-91
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• 2022

Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquid-chromatography-tandem-mass-spectrometric method (LC-MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 ㎍/g. The intra- and inter-day deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 - 64.86 ㎍/g and 0.25 - 63.99 ㎍/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.

• Pediatric Gastroenterology, Hepatology & Nutrition
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• v.11 no.2
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• pp.223-225
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• 2008

Rhododendron species is one of the largest and most diverse genera in the plant kingdom, comprising over 800 species and existing all over the globe. Grayanotoxin intoxication is caused by ingestion of honey and flowers. Grayanotoxin exists in honey, flowers, pollen, and nectar of the Rhododendron species. Grayanotoxin-intoxicated patients may present with nausea, vomiting, dizziness, weakness, hypotension, bradycardia, and syncope for several hours. We report a case of grayanotoxin intoxication associated with mental changes. A 9-year-old male presented with impaired consciousness and delirium 26 hours after eating about 10 rhododendron sclippenbachii flowers. A brain MRI and EEG were normal. Parenteral fluids were administered and these symptoms resolved completely in 17 hours.

• Applied Biological Chemistry
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• v.46 no.2
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• pp.144-149
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• 2003

Extracts were obtained from the flower of Rhododendro yedoense var. poukhanense. (7 kg) in 80% aqueous MeOH and successively fractionated with solvent of EtOAc, n-BuOH and $H_2O$, successively. Silica gel and ODS column chromatographies of the EtOAc and n-BuOH fractions were repeatedly carried out by using the various solvent systems to give five terpenoids. Chemical structures of the isolated terpenoids were determined as $2{\alpha},3{\beta}-dihydroxylolean-12-ene$ (1), ursolic acid (2), grayanotoxin IV (3), grayanotoxin I (4) and grayanotoxin III (5) based on the interpretation of several spectral data including 2D-NMR such as $^1H-^1H\;COSY$, HMQC and HMBC.

• Korean Journal of Veterinary Service
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• v.40 no.4
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• pp.277-280
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• 2017

A 3 year-old black goat was presented to Animal and Plant Quarantine agency for diagnosis in June, 2017. She was intaken feed with Rhododendron schlippenbachii the day before death. The clinical signs included loss of appetite, lethargy, hypersalivation, astasia, yelling. At necropsy, foamy discharge were observed in the airway. Histologically, foreign body, eosinphil and macrophges was observed in alveolar lumen of lung. Grayanotoxin derived from Rhododendrons was detected in ruminal contents. Based on the pathological and toxine examination, we diagnosed this case as grayanotoxin poisoning in a black goat.

• Korean Journal of Food Science and Technology
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• v.40 no.1
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• pp.8-14
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• 2008

This study was performed to establish analysis methods, and evaluated for grayanotoxin in domestic/foreign honey and wild honey. The molecular weight of grayanotoxins I, II and III, excluding grayanotoxin III that has been commercialized, were analyzed by LC-MS/MS. Then, the molecular structure of grayanotoxins I and II were analyzed by NMR. A total 111 samples (25 Korean honey, 21 Korean wild honey, 13 Korean honeycomb honey, 44 foreign honey, 8 foreign wild honey) were examined to determined whether or not each sample contained grayanotoxins I, II, and III. The honey samples were mixed with methanol and loaded into a tC18 cartridge, the filtrate was diluted with water, and the mixture was then analyzed by ESI triple-quadrupole LC-MS/MS. Grayanotoxins were only found in the foreign wild honey and were not detected in Korean honey, Korean honeycomb honey, or Korean wild honey. Three of the samples contained grayanotoxin I, II, and III, and one sample contained only grayanotoxins I and III. The lowest level for grayanotoxin I was 3.13 ${\pm}$ 0.00 mg/kg, and the highest level was 12.93 ${\pm}$ 0.01 mg/kg. The levels of grayanotoxin II were 0.84 ${\pm}$ 0.01 mg/kg, 0.92 ${\pm}$ 0.00 mg/kg and 1.08 ${\pm}$ 0.01 mg/kg, respectively. The lowest level of grayanotoxin III was 0.25 ${\pm}$ 0.01 mg/kg and the highest level was 3.29 ${\pm}$ 0.74 mg/kg. Through this study, safety management for foreign wild honey has been enabled.

• Journal of The Korean Society of Clinical Toxicology
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• v.10 no.1
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• pp.37-40
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• 2012

Honey is produced by bees from nectar collected from nearby flowers. Sometimes, honey produced from the Rhododendron species is contaminated by Grayanotoxin (GTX) in Nepal and other countries. There have been reports of GTX intoxication, also known as 'mad honey disease', from honey produced in countries other than Korea. The importation of wild honey has been prohibited by the Korean Food and Drug Administration since 2005, yet it is still distributed within Korea by the occasional tourist. We report a case of GTX intoxication from contaminated honey which included the symptoms of nausea, vomiting, general weakness, dizziness, blurred vision, hypotension and sinus bradycardia. By means of infusion with normal saline and atropine sulfate, the patient's condition fully recovered within 8 hours of hospital admission, and she was discharged without any complications.

• Journal of The Korean Society of Clinical Toxicology
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• v.7 no.2
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• pp.180-182
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• 2009

It is well known that Rhododendron sclippenbashii contains the toxic material grayanotoxin. So, Koreans do not eat it, but they do eat azalea although it contains grayanotoxin. That is why there have been no reports about Rhododendron sclippenbashii intoxication after ingesting it intentionally, not accidentally. In this case, the patient was admitted to the emergency room with several toxic symptoms after intentionally consuming 50 blossoms of Rhododendron sclippenbashii to get rid of thirst. Treatment with saline infusion and atropine was successful and the outcome was favorable enough in this case to produce a complete cure without any sequelae at discharge. But toxic symptoms were seen for 24 hours, although the symptoms usually fade in 9 hours. Therefore, we should carefully treat and observe, for over 24 hours, the patient who intentionally ingests about 50 blossoms of Rhododendron sclippenbashii.

• Natural Product Sciences
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• v.4 no.2
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• pp.68-71
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• 1998

Three grayanane diterpenoids (1-3) were isolated from Pieris formosa. 1 was identified as a new natural product and 2 and 3 as known grayanoside C and grayanotoxin XVIII on the basis of spectral analysis.

• Archives of Pharmacal Research
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• v.10 no.3
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• pp.169-172
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• 1987

From the leaves of Rhododendron brachycarpum, rhododendrin, grayanotoxin I and guaijaverin were isolated and characterized by spectral data.

• Journal of The Korean Society of Clinical Toxicology
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• v.4 no.2
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• pp.143-146
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• 2006

Historically, the common folk have made use of various wild herbs for both food and medicinal purposes. However, the misuse of these wild herbs can lead to adverse consequences, including severe poisoning in some cases. In cases of poisoning from wild herbs, patients can exhibit a variety of symptoms depending on the herbs involved, which in addition to gastrointestinal symptoms may include hemodynamic alteration and abnormal neurologic signs. In the present case, two patients were admitted to the emergency room with symptoms of toxicity after consuming Rhododendron brachycarpum liquor. Rhododendron brachycarpum and other wild herbs contain the toxic material grayanotoxin. Because of its serious toxic symptoms, great caution must be exercised in using rhododendrons for food and medicinal purposes.