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Title: Določanje neonikotinoidov v medu in cvetnem prahu s HPLC-DAD in TLS detekcijo Authors: ID Mejač, Irena (Author) ID Franko, Mladen (Mentor) More about this mentor... Files: http://www.ung.si/~library/diplome/OKOLJE/8Mejac.pdf   8Mejac.pdf (713,06 KB) MD5: DC7E43FD595B7B6332D66DB5626F4891   Language: Slovenian Work type: Undergraduate thesis Typology: 2.11 - Undergraduate Thesis Organization: FZO - Faculty of Environmental Sciences Abstract: Razvili smo kromatografsko metodo HPLC za določevanje nekaterih neonikotinoidov (imidakloprid, tiametoksam, acetamiprid in tiakloprid) v vzorcih medu in cvetnega prahu. Neonikotinoide smo iz vzorcev medu ekstrahirali z ekstrakcijo tekoče-tekoče v diklorometan, iz cvetnega prahu pa z ekstrakcijo trdno-tekoče v diklorometan:aceton. Z dodatkom standardnih raztopin neonikotinoidov vzorcem medu in cvetnega prahu pred ekstrakcijo smo pripravili umeritvene premice z visokimi regresijskimi koeficienti (> 0,994) v koncentracijskem območju 0,1-5 mg/kg. Vzorce smo analizirali na reverzno-fazni kromatografski koloni C[sub]18 ob uporabi izokratične metode elucije z acetonitrilom:10mM amonijevim acetatom (3:7, v/v) in pretoka 1 mL/min. Za detekcijo neonikotinoidov po kromatografski ločbi smo uporabili spektrofotometrično metodo z diodno matriko DAD in spektrometrijo s toplotnimi lečami TLS. Zaradi različnih absorbcijskih spektrov posameznih neonikotinoidov smo v primeru DAD določevali insekticide pri štirih valovnih dolžinah (254, 270, 245 in 242 nm), v primeru TLS pa smo lahko uporabili le valovno dolžino vzbujevalnega laserja 244 nm. Doseženi izkoristki ekstrakcij iz medu so bili med 76 in 83 % za acetamiprid, tiakloprid in tiametoksam ter 99 % za imidakloprid. Relativni standardni odmiki pri koncentraciji 1 mg/kg in petih ponovitvah so bili v območju 15-38 %. Meje zaznavnosti so bile 50 [mi]g/kg za imidakloprid, 100 [mi]g/kg za tiametoksam in acetamiprid ter 250 [mi]g/kg za tiakloprid. Izkoristki ekstrakcij iz cvetnega prahu so bili občutno nižji, v območju 45-54 %, in so omogočali doseganje meje zaznavnosti 500 [mi]g/kg za vse štiri insekticide. Z metodo HPLC-TLS smo za primer standardnih raztopin neonikotinoidov dosegli meje zaznavnosti v območju 10 [mi]g/kg za acetamiprid do 25 [mi]g/kg za tiametoksam in imidakloprid in s tem znižanje vrednosti LOD v primerjavi s HPLC-DAD metodo. Keywords: diplomske naloge, ekstrakcija, med, cvetni prah, kromatografija Place of publishing: Nova Gorica Publisher: I. Mejač Year of publishing: 2006 Number of pages: IV, 54 str. PID: 20.500.12556/RUNG-577  COBISS.SI-ID: 536315  UDC: 504 NUK URN: URN:SI:UNG:REP:DMUP8GXK Publication date in RUNG: 15.10.2013 Views: 8357 Downloads: 488 Metadata:    Cite this work Plain text BibTeX EndNote XML EndNote/Refer RIS ABNT ACM Ref AMA APA Chicago 17th Author-Date Harvard IEEE ISO 690 MLA Vancouver : MEJAČ, Irena, 2006, Določanje neonikotinoidov v medu in cvetnem prahu s HPLC-DAD in TLS detekcijo [online]. Bachelor’s thesis. Nova Gorica : I. Mejač. [Accessed 19 March 2025]. Retrieved from: https://repozitorij.ung.si/IzpisGradiva.php?lang=eng&id=577 Copy citation

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A HPLC chromatographic method combined with liquid-liquid extraction into dichloromethane and solid-liquid extraction into acetone:dichloromethane was developed for simultaneous determination of some neonicotinoids (imidacloprid,thiamethoxam, acetamiprid and thiacloprid) in pollen and commercial honey samples. Calibration curves with high regression coefficients(> 0.994) were prepared in the 0.1-5 mg/kg concentration range by adding appropriate amounts of neonicotinoids to honey or pollen samples before the extraction. Samples were analyzed on a reverse-phase C[sub]18 chromatographic column using isocratic elution with acetonitrile:10 mM ammonium acetate (3:7, v/v) as eluent, and 1 mL/min flow rate. Detection of neonicotinoids was performed by DAD diode-array spectrophotometric method or by thermal lens spectrometry (TLS). Due to differences in absorption spectra of studied insecticides all chromatograms were recorded at four wavelengths (254, 270, 245 and 242 nm) in case of DAD. For TLS measurements only the wavelength of the excitation laser (244 nm) was used. Recoveries from honey were between 76 and 83 % for acetamiprid, thiacloprid, and thiametoxam, and 99% for imidacloprid. Relative standard deviations of five determinations in honey fortified at 1 mg/kg level were in the range of 15-38 % depending on the insecticide. The achieved limits of detection (LOD) were from 50 [mu]g/kg for imidacloprid to 100 [mu]g/kg for thiametoxam and acetamiprid, and 250 [mu]g/kg for thiacloprid. In case of pollen recoveries were significantly lower and ranged from 45-54 %, while the achieved LODs were at 500 [mu]g/kg for all four insecticides. In case of HPLC-TLS only standard neonicotinoid solutions were analyzed, and the LOD values ranging from 10 [mu]g/kg for acetamiprid up to 25 [mu]g/kg for thaimethoxam and imidacloprid were achieved. This represents an improvement compared to the HPLC-DAD method.

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