Simultaneous Determination of Ergot Alkaloids in Swine and Dairy Feeds Using Ultra High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Ergot alkaloids (EAs) are mycotoxins mainly produced by the fungus Claviceps purpurea. EAs are known to affect the nervous system and to be vasoconstrictors in humans and animals. This work presents recent advances in swine and dairy feeds regarding 11 major EAs, namely ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine, ergosinine, ergotaminine, ergocorninine, ergocryptinine, and ergocristinine. A reliable, sensitive, and accurate multiple mycotoxin method, based on extraction with a Mycosep 150 multifunctional column prior to analysis using UHPLC-MS/MS, was validated using samples of swine feed (100) and dairy feed (100) for the 11 targeted EAs. Based on the obtained validation results, this method showed good performance recovery and inter-day and intra-day precision that are in accordance with standard criteria to ensure reliable occurrence data on EA contaminants. More than 49% of the swine feed samples were contaminated with EAs, especially ergocryptine(-ine) (40%) and ergosine (-ine) and ergotamine (-ine) (37%). However, many of the 11 EAs were not detectable in any swine feed samples. In addition, there were contaminated (positive) dairy feed samples, especially for ergocryptine (-ine) (50%), ergosine (-ine) (48%), ergotamine (-ine), and ergocristine (-ine) (49%). The mycotoxin levels in the feed samples in this study almost complied with the European Union regulations.

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Розробка та оцінка придатності методу з визначення антибіотиків у молоці за допомогою рідинної хроматографії високого тиску - тандемної мас-спектрометрії (UPLC-MS-MS)

Ukrainian Journal of Ecology ◽

10.15421/2017_162 ◽

2017 ◽

Vol 7 (4) ◽

pp. 569-575

Author(s):

O. V. Bayer ◽

O. S. Yaremchuk ◽

L. V. Shevchenko ◽

V. M. Mykhalska

Keyword(s):

High Performance ◽

Screening Method ◽

Penicillin G ◽

Screening Methods ◽

The European Union ◽

Chromatography Tandem Mass Spectrometry ◽

Council Directive ◽

Residual Amount ◽

Liquid Chromatography Tandem Mass

<p>On the basis of the conducted research, validation of the method for the determination of sulfonamides and antibiotics in milk by screening method was developed and conducted by LC / MS / MS. It has been confirmed that a method determination by ultra-high-performance liquid chromatography–tandem mass spectrometry (UPLC / MS / MS) is more sensitive and selective. Validation of the method was carried out in accordance with the Decision of the European Commission 2002/657 / EC of 12 August 2002, which ensures the implementation of Council Directive 96/23 / EC concerning the effectiveness of analytical methods and the interpretation of results, and in accordance with the recommendations of the reference laboratories of the European Union CRLs of 20/1/2010 on the assessment of the suitability of screening methods for the determination of veterinary drugs. It is proved that the adapted method for the determination of sulfonamides and antibiotics is sensitive and according to parameters meets the European requirements. This method is fast enough, practical and universal, since it allows simultaneous examination of about 70 antibacterial drugs at the same time in milk.</p><p>It has been established that the method of determining the residual amount of sulfonamides and antibiotics by the UPLC / MS / MS is suitable for the investigation of milk on the content of the following drugs: sulfaguanidine, sulfacetamide, sulfapiridine, sulfadiazine, sulfamethoxazole, sulfathiazole, sulfamethazine, sulfamethizole, sulfabenzamide, sulfaquinoxaline, sulfadoxine, sulfadimetoxin, sulfanilamide, trimethoprim, sulfamonomethoxine, sulfamethoxypyridazine, sulfachlorpyridazine, sulfamoxol, dapsone, amoxicillin, ampicillin, penicillin G, penicillin V, oxacillin, cloxacillin, nafcillin, dicloxacillin, cefalonium, cefazolin, cefoperazon, cefquinome, cefapirin, ceftiofur, cefalexin, norfloxacin, enrofloxacin, ciprofloxacin, marbofloxacin, difloxacin, danofloxacin, sarafloxacin, flumekvin, oxolinic acid, nalidixic acid, oxytetracycline, chlortetracycline, tetracycline, doxycycline, epi-oxytetracycline, epi-tetracycline, epi-chlortetracycline, streptomycin, dihydrostreptomycin, gentamicin, kanamycin, apramycin, paromomycin, lincomycin, spectinomycin, tilmycosin, erythromycin, josamycin, spiramycin, tylosin, tiamulin, colistin, gamitromycin, tulatromycin. In assessing the suitability of the method, the MS / MS detection parameters are set and the validation characteristics are determined.</p>

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Simultaneous Determination of Multiple Mycotoxins in Swine, Poultry and Dairy Feeds Using Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

Toxins ◽

10.3390/toxins12040253 ◽

2020 ◽

Vol 12 (4) ◽

pp. 253 ◽

Cited By ~ 1

Author(s):

Kraiwut Nualkaw ◽

Saranya Poapolathep ◽

Zhaowei Zhang ◽

Qi Zhang ◽

Mario Giorgi ◽

...

Keyword(s):

Mass Spectrometry ◽

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

High Performance ◽

Tandem Mass ◽

Chromatography Tandem Mass Spectrometry ◽

Liquid Chromatography Tandem Mass ◽

Feed Samples

A reliable, sensitive and accurate multiple mycotoxin method was developed for the simultaneous determination of 17 mycotoxins in swine, poultry and dairy feeds using stable isotope dilution (13C-ISTD) and (ultra)-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A simple QuEChERS-based method (quick, easy, cheap, effective, rugged and safe) was developed consisting of soaking with a solution of 1% formic acid followed by extraction with acetonitrile, clean-up with C18 sorbent and finally adding 13C-ISTD before the UHPLC-MS/MS analysis. The chromatographic condition was optimized for separation and detection of the 17 mycotoxins using gradient elution. The method’s performance complied with the SANTE/11813/2017 standard and had mean recovery accuracies in the range 70%–120% and precision testing of % relative standard deviation (RSD) ≤ 20%. The limit of detection and limit of quantification values ranged from 0.25 to 40.0 ng/g and 0.5 to 100.0 ng/g, respectively. Finally, the method was applied to analyze feed samples, with the results showing that fumonisins, zearalenone, aflatoxin B1 and deoxynivalenol were the most prevalent mycotoxins contaminating the feed samples.

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