Uncertainties in the determination of pyrrolizidine alkaloid levels in naturally contaminated honeys and comparison of results obtained by different analytical approaches

The contamination of honey with hepatotoxic pyrrolizidine alkaloids (PAs) is a well-known hazard for food safety. While management strategies and controls of the honey industry aim to reduce the PA levels, uncertainties remain with regard to the safety of regionally produced and marketed honey. In addition, a previous study showed large differences of results obtained after various periods of storage and apparent differences between the analytical results of different laboratories. Therefore, this study aimed at examining these uncertainties by monitoring the impact of storage on the PA and PA N-oxide (PANO) content of two freshly harvested honeys and on possible demixing effects caused by pollen settling. Additionally, three analytical approaches – target analysis with matrix-matched calibration or standard addition and a sum parameter method – were applied for a comparative analysis of 20 honeys harvested in summer 2016. All samples originated from Schleswig-Holstein in Northern Germany where the PA plant Jacobaea vulgaris is currently observed on a massive scale. The results of the time series analyses showed that PANO levels markedly decreased within a few weeks and practically reached the LOD 16 weeks after harvest. Tertiary PAs, by contrast, remained stable and did not increase as a consequence of PANO decrease. The experiments on a putative demixing, which may result in a heterogeneous distribution of PAs/PANOs, revealed that there was no such effect during storage of up to 12 weeks. A comparison of the PA/PANO levels obtained by different analytical approaches showed that in some cases the sum parameter method yielded much higher levels than the target approaches, whereas in other cases, the target analysis with standard addition found higher levels than the other two methods. In summary, the results of this study highlight uncertainties regarding the validity and comparability of analytical results and consequently regarding health risk assessment.     

Quantitative UPLC‐MS/MS analysis of chlorogenic acid derivatives in antioxidant fractionates from dandelion (Taraxacum officinale) root

While qualitative studies have identified chlorogenic acids in antioxidant extracts, particularly ethyl acetate‐derived extracts, of Taraxacum officinale, quantitative analysis of these phenolic compounds remains largely unreported for this species. In this study, bioactivity‐guided fractionation of an antioxidant crude ethyl acetate extract (DPPH = 295.481 ± 0.955 mg TE g^?1 extract) from T. officinale root resulted in a number of reverse‐phase fractions that demonstrated high antioxidant activity (DPPH = 1058.733–1312.136 mg TE g^?1 extract), stronger than that of the synthetic antioxidant Trolox^®. UPLC‐MS/MS screening of these fractions for the presence of selected mono‐ and di‐caffeoylquinic acids revealed large quantities of 1,5‐dicaffeoylquinic acid present in several fractions (853.052–907.324 μg mg^?1), respectively. Due to the antioxidant potency and high levels of 1,5‐dicaffeoylquinic acid observed in these fractions, it was concluded that specifically this chlorogenic acid derivative is a major contributor to the antioxidant efficacy of dandelion root.     

Bioactive compounds and antioxidant activities of the Korean lotus leaf (Nelumbo nucifera) condiment: volatile and nonvolatile metabolite profiling during fermentation

Recent studies have shown that lotus (Nelumbo nucifera) leaf has various pharmacological effects. However, there have been no scientific investigations into these leaves as a fermented crude liquid. This study compared the in vitro antioxidant capacity of lotus leaf‐fermented broth (LLFB) with that of 57° Brix sugar broth (SB) as a control over a period of 6 months based on 1,1‐diphenyl‐2‐picrylhydrazyl radical scavenging activity, ferric ion reducing power, superoxide dismutase‐like activity, tyrosinase inhibition and nitrite scavenging activity. The dominant species during fermentation process were Leuconostoc lactis and Saccharomyces cerevisiae for LLFB. A total of thirty‐six metabolites such as alkaloids, fatty acids, organic acids, phenolics, sugar and sugar derivatives, ethyl esters and monoterpenoids differed between SB and LLFB using gas chromatography–mass spectrometry. Meanwhile, nine volatile compounds in LLFB contributed pleasant, slightly sweetish and fruity odour of condiment and sensory evaluation score of 4.06 ± 1.52 in the proportion of 1:9 LLFB/water.     

Comparison of two Analytical Methods (ELISA and LC-MS/MS) for Determination of Aflatoxin B1 in Corn and Aflatoxin M1 in Milk

The aim of this paper is to assess the closeness of agreement between results of ELISA and LC-MS/MS methods for determination of aflatoxin B₁ in corn and aflatoxin M₁ in milk. Samples of corn (n=100) and milk (n=250) were simultaneously analyzed using ELISA and LC-MS/MS methods, after the severe drought that affected Serbia in summer 2012 resulting in occurrence of aflatoxin B1 in corn and aflatoxin M₁ in milk. Regression analysis showed higher level of agreement between aflatoxin B₁ samples (R²=0.994), compared to aflatoxin M₁ samples (R²=0.920). However, both techniques were satisfactory in meeting the requirements for official control purposes.     

微机械热对流倾角仪温度补偿技术研究

介绍了微机械热对流倾角仪的工作原理和结构设计,利用有限元分析软件,计算了在不同倾斜状态下二维密闭腔中点热源引起的对流场和温度场,提出了环境温度对热对流倾角仪影响的模型。根据仿真结果,在电路中增加了加热丝恒定温度控制电路,建立了基于软件的环境温度补偿算法,实现了对温度影响的补偿。经测试,环境温度从-40℃变化到60℃时,倾角仪0°输入的温度稳定性为0.07°,10°输入的温度稳定性为0.02°。     

A Study on NMR and GC/MS Spectra of the Isomers of Linear Hexyl Naphthalene

The GC/MS and NMR analysis of the reaction products of naphthalene with 1-bromohexane were reported. The products obtained were suggested to have six isomers of linear hexylnaphthalene and the structure of each isomer was determined by GC/MS and NMR spectra. For the first time, the unique chemical shift data were obtained. The content of each isomer calculated by ¹H NMR and ¹³C NMR spectra was consistent with that by GC/MS spectra, which confirmed the accuracy of NMR data.     

选煤综合网络管理信息系统的设计与实现

从中国煤炭加工利用协会的实际需要出发，用POWERBUILDER7．0和MS SQL Server2000开发基于客户机/服务器体系结构的选煤综合网络管理信息系统。本系统设计具有友好的用户界面，可以方便地输入数据、编辑表格，还有打印、数据统计与记录查询等功能。     

玫瑰油化学成分分析和电子香味分析

为区分不同档次的玫瑰油,利用GC/MS法对高、中档玫瑰油进行了化学成分的定性和定量分析,分别鉴定出63和72种化合物。并对这2种玫瑰油和1种待测样品进行了电子香味扫描,确定电子鼻在玫瑰油档次辨别中的作用。