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Simultaneous determination of pyrrolizidine and tropane alkaloids in honey by liquid chromatography–mass spectrometry
2022
Kowalczyk, Ewelina | Kwiatek, Krzysztof
Pyrrolizidine alkaloids (PAs) and tropane alkaloids (TAs) are natural contaminants of honey and respectively hepatoxic and neurotoxic compounds. Because honey is a popular constituent of the human diet, it is relevant to warrant the safety of the product. For that reason, a method for simultaneous determination of PAs and TAs in honey based on liquid chromatography– mass spectrometry was developed. The analytical protocol used sulphuric acid extraction and solid-phase extraction purification. The developed procedure was subjected to validation in terms of linearity, selectivity, repeatability, reproducibility, limits of quantification and determination, matrix effect and uncertainty. A total of 29 honey samples were analysed for the determination of PAs and TAs. All the evaluated validation parameters fulfilled the requirements of European Commission Decision 2002/657/EC. At least one of the monitored alkaloids was determined in 52% of the samples. Among the most abundant alkaloids were echimidine, intermedine and lycopsamine. The total PA concentrations ranged from 2.2 to 147.0 μg kg⁻¹. Contrastingly, none of the monitored TAs was detected in the analysed samples. An assessment of the dietary exposure to PAs from the consumption of the contaminated honeys showed that three of them would pose a risk to consumers, especially if they were children. A sensitive method suitable for simultaneous determination of PAs and TAs in honey was developed and validated. The analysis of 29 honey samples for PAs and TAs revealed that honey destined for retail could pose a risk to consumers.
Show more [+] Less [-]Bootstrap simulation for quantification of uncertainty in risk assessment
2007
Chang, K.Y. (Ministry of Agriculture and Forestry, Gwacheon, Republic of Korea) | Hong, K.O. (Ministry of Agriculture and Forestry, Gwacheon, Republic of Korea) | Pak, S.I. (Kangwon National University, Chuncheon, Republic of Korea), E-mail: paksi@kangwon.ac.kr
The choice of input distribution in quantitative risk assessments modeling is of great importance to get unbiased overall estimates, although it is difficult to characterize them in situations where data available are too sparse or small. The present study is particularly concerned with accommodation of uncertainties commonly encountered in the practice of modeling. The authors applied parametric and non-parametric bootstrap simulation methods which consist of re-sampling with replacement, in together with the classical Student-t statistics based on the normal distribution.
Show more [+] Less [-]Estimation of uncertainty for the determination of residual flubendazole in pork
2007
Kim, M.K. (National Veterinary Research and Quarantine Service, Anyang, Republic of Korea), E-mail: kimmk@nvrqs.go.kr | Park, S.J. (National Veterinary Research and Quarantine Service, Anyang, Republic of Korea) | Lim, C.M. (National Veterinary Research and Quarantine Service, Anyang, Republic of Korea) | Cho, B.H. (National Veterinary Research and Quarantine Service, Anyang, Republic of Korea) | Kwon, H.J. (National Veterinary Research and Quarantine Service, Anyang, Republic of Korea) | Kim, D.G. (National Veterinary Research and Quarantine Service, Anyang, Republic of Korea) | Chung, G.S. (National Veterinary Research and Quarantine Service, Anyang, Republic of Korea)
Measurement uncertainty could play an important role in the assessment of test results in laboratories and industries. We investigated measurement uncertainties possibly included in determination of flubendazole, a benzimidazole anthelmintic, in pork by HPLC. The concentration of flubendazole was 62.69 ng/g in a sample of pork. Uncertainty was estimated in the analytical procedure of flubendazole. A model equation was made for determination of flubendazole in pork. The four uncertainty components such as weight of sample, volume of sample, calibration curve, and recovery were selected to estimate measurement uncertainties.
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