Migration behavior and dietary exposure risk assessment of pesticides residues in honeysuckle (Lonicera japonica Thunb.) based on modified QuEChERS method coupled with tandem mass spectrometry.

The honeysuckle was widely appreciated as tea beverage owing to the biological activities and the unique aroma and flavor. It is in urgent requirement to explore the migration behavior and dietary exposure as the pesticide residues would bring about potential risks through honeysuckle intake. The optimized QuEChERS procedure coupled with the HPLC-MS/MS and GC-MS/MS methods were employed to determine 93 pesticide residues of seven classifications including carbamates, pyrethroid, triazoles, neonicotinoids, organophosphorus, organochlorine, and others for 93 honeysuckle samples from four primary production bases. As a result, 86.02% of the samples were contaminated by at least one pesticide. Unexpectedly, the banned pesticide of carbofuran was also identified. The migration behavior of metolcarb was the highest, whereas thiabendazole contributed less risk to the infusion with relative lower transfer rate. Both the chronic and acute exposure yielded low risk for human health with five high risk pesticides of dichlorvos, cyhalothrin, carbofuran, ethomyl, and pyridaben. Besides, this study provides foundation of dietary exposure risk assessment for honeysuckle and other likewise products.

The dissipation, processing factors, metabolites, and risk assessment of pesticides in honeysuckle from field to table.

Globally, honeysuckle is consumed as a food and administered as a medicinal agent. However, pesticide residues in honeysuckle limit its application and development of the honeysuckle industry, affecting food safety and endangering human health. Here, the degradation kinetics of 11 typical pesticides, including insecticides, fungicides, and an acaricide, in honeysuckle were investigated. The half-lives of pesticides in Henan and Liaoning fields were 1.90-4.33 and 2.05-4.62 d, respectively. The processing factors (PFs) of these pesticides after oven, sun, and shade drying ranged from 3.52 to 11.2. After decocting, the PFs of the pesticides were <1. Twenty degradation products were identified using ultra high performance liquid chromatography-quadrupole time-of-flight mass spectrometry, and pathways were proposed based on drying and decoction. The ecotoxicities of the degradation products were evaluated using the Toxicity Estimation Software Tool. Finally, the acute hazard indices of these pesticides, as determined via dietary exposure assessment combined with the PFs, were 0.227 and 0.911 for adults and children, respectively. Thus, special populations, such as children, require particularly careful risk control in terms of dietary exposure.

Analysis of heavy metal content in edible honeysuckle (Lonicera japonica Thunb.) from China and health risk assessment.

Honeysuckle is a commonly used medicine for health care and treatment. To detect heavy metal pollution in honeysuckle from China and quantify the health risk of heavy metal via dietary intake, the Pb, Cd, Cr, As, Hg, Ni, Mn, Cu, and Zn contents in honeysuckle samples were determined by ICP-MS. The dissolution rate of heavy metals in honeysuckle was measured by decoction and soaking. The hazard quotient (HQ) and total hazard index (HI) were used to evaluate the noncarcinogenic risk of nine heavy metals in honeysuckle, and the carcinogenic risks of Cd and As were evaluated using the carcinogen risk. Cd exhibited the maximum permissive limit standard-exceeding rate (40.2%) in honeysuckle, followed by Cu (37.6%) and Pb (8.5%). As and Hg did not exceed the standard values, and Cr, Ni, Mn, and Zn had no limits. In a decoction fluid after 30 min of boiling, the transfer rates of Pb, Cd, As, Ni, Mn, Cu, and Zn ranged from 11.9% to 19.9%, whereas that of Cr was low (1.0%). In a soaking fluid, the transfer rates ranged from 17.0% to 56.9%; no transfer rate was detected for Hg in neither the decoction fluid nor the soaking fluid. In addition, the 95th percentile Rs of As and Cd in honeysuckle were 5.93 × 10-6 and 8.12 × 10-5, respectively. The carcinogenic risk of Cd at 56.99th percentile reached the threshold set by the World Health Organization (1.0 × 10-5). The results showed that intake of Pb, Cd, Cr, As, Hg, Ni, Mn, Cu, and Zn by the human body through honeysuckle could not cause noncarcinogenic damage. The element As had no carcinogenic risk, but Cd had a carcinogenic risk to a certain extent.

[Residual status and risk assessment of forbidden and restricted pesticides of organophosphorus in Loincerae Japonicae Flos].

This paper reports the residual status of forbidden and restricted pesticides of organophosphorus in Loincerae Japonicae Flos to provide reference for the risk control and the formulation of maximum residue limits of the flower. A method for the determination of residues of 23 forbidden and restricted pesticides of organophosphorus was established, and 64 collected samples were tested. Then a risk assessment based on the maximum residue limit was carried out. Results showed that the detection rate of samples was 58%. 6 of 23 pesticides were detected and the ratio was chlorpyrifos 41%, omethoate 23%, triazophos 11%, isofenphos-methyl 6.3%, methamidophos 1.6%, isocarbophos 1.6%, respectively. And the median of pesticide residues in the positive samples was chlorpyrifos 0.037 mg·kg⁻¹, omethoate 0.043 mg·kg⁻¹, triazophos 0.030 mg·kg⁻¹, isofenphos-methyl 0.18 mg·kg⁻¹, methamidophos 0.041 mg·kg⁻¹, isocarbophos 0.041 mg·kg⁻¹, respectively. In the samples with pesticide residues, the residue amount of methamidophos and isocarbophos was lower than the theoretical maximum residue limit, and the residue amount of chlorpyrifos, isofenphos-methyl, triazophos were higher than it individually, while, all the residue amount of omethoate was higher than it. According to the assessment result of theoretical maximum residue limit, it is suggested that relevant departments should accelerate the formulation of the maximum residue limit standard, and strengthen the supervision of the use of forbidden and restricted pesticides of organophosphorus in Loincerae Japonicae Flos.

Assessment of anti-inflammatory properties of extracts from Honeysuckle (Lonicera sp. L., Caprifoliaceae) by ATR-FTIR spectroscopy.

Inflammation is a hallmark of some of today's most life-threatening diseases such as arteriosclerosis, cancer, diabetes and Alzheimer's disease. Herbal medicines (HMs) are re-emerging resources in the fight against these conditions and for many of them, anti-inflammatory activity has been demonstrated. However, several aspects of HMs such as their multi-component character, natural variability and pharmacodynamic interactions (e.g. synergism) hamper identification of their bioactive constituents and thus the development of appropriate quality control (QC) workflows. In this study, we investigated the potential use of Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) spectroscopy as a tool to rapidly and non-destructively assess different anti-inflammatory properties of ethanolic extracts from various species of the Genus Lonicera (Caprifoliaceae). Reference measurements for multivariate calibration comprised in vitro bioactivity of crude extracts towards four key players of inflammation: Nitric oxide (NO), interleukin 8 (IL-8), peroxisome proliferator-activated receptor ß/δ (PPAR ß/δ), and nuclear factor kappa-light-chain-enhancer of activated B-cells (NF-κB). Multivariate analysis of variance (MANOVA) revealed a statistically significant, quantitative pattern-activity relationship between the extracts' ATR-FTIR spectra and their ability to modulate these targets in the corresponding cell models. Ensemble orthogonal partial least squares (OPLS) discriminant models were established for the identification of extracts exhibiting high and low activity with respect to their potential to suppress NO and IL-8 production. Predictions made on an independent test set revealed good generalizability of the models with overall sensitivity and specificity of 80% and 100%, respectively. Partial least squares (PLS) regression models were successfully established to predict the extracts' ability to suppress NO production and NF-κB activity with root mean squared errors of cross-validation (RMSECV) of 8.7% and 0.05-fold activity, respectively.

A reversed-phase/hydrophilic interaction mixed-mode C18-Diol stationary phase for multiple applications.

A mixed-mode chromatographic packing material, C18 and diol groups modified silica (C18-Diol), was prepared with controllable hydrophobicity and hydrophilicity. It demonstrated excellent aqueous compatibility and stability in aqueous mobile phase; compared to the traditional C18 column, improved peak shape of basic analytes was also obtained. Additionally, it exhibited both reversed-phase liquid chromatographic (RPLC) and hydrophilic interaction chromatographic (HILIC) performance; the analyte separation scope was thus enlarged, demonstrated by simultaneous separation of twenty acids, bases and neutrals. More interestingly, a novel on-line two-dimensional liquid chromatography on the single column (2D-LC-1C) was established by modifying the high performance liquid chromatographic instrument only with the addition of an extra six-port two-position valve. The early co-eluted components of the extract of Lonicera japonica on the 1st-dimension (RPLC) were collected for the online re-injection to the 2nd-dimension (HILIC) by conveniently varying the mobile phase components. Six more peaks were obtained. The established system was simple, easy operation and low cost, which had advantages in analyzing complicated samples.