基质分散固相萃取-液相色谱-串联质谱法检测动物源性食品中硝基咪唑药物及其代谢物

建立了基质分散固相萃取-液相色谱-串联质谱（dSPE-LC-MS/MS）定量检测4种动物源性食品基质中硝基咪唑类药物及其代谢物的方法。样品（2.0 g）用乙酸乙酯提取后浓缩,经正己烷脱脂、50 mg乙二胺-N-丙基硅烷（PSA）吸附剂吸附净化后,过0.22 μm亲水聚四氟乙烯（PTFE）滤膜。采用C18柱分离,在电喷雾电离（ESI）源和选择反应监测（SRM）模式下检测,基质匹配内标法定量。在0.5~20.0 μg/L范围内,硝基咪唑类药物及其代谢物呈现良好的线性关系,相关系数（r²）>0.99;方法的检出限为0.1~0.5 μg/kg;在1.0、3.0和10.0 μg/kg的加标水平下,硝基咪唑类药物及其代谢物的回收率为84.2%~120.8%,相对标准偏差为2.0%~16.2%（n=6）。该法准确、快速,成本低,易操作,能够满足动物源性食品中硝基咪唑类药物及其代谢物残留的监测要求。     

Tracing changes in the diet and habitat use of black-tailed godwits in Western France,using a stable isotope approach

Western France is at the crossroads of the migratory routes of two subspecies of black-tailed godwit, Limosa limosa. After leaving Iceland, the godwit L.l. islandica Icelandic black-tailed godwit (IBTG) winters on the coast of western Europe, while the continental black-tailed godwit (CBTG) L.l. limosa can stop in France when migrating between Iberia or Africa and their main breeding grounds in the Netherlands. In this study, we analysed δ¹⁵N and δ¹³C from flight feathers and whole blood throughout the non-breeding period to trace variations in habitat use for both subspecies on the western French coast. Adults and juveniles of IBTG adopt the same feeding habitats as soon as they arrive in the study area, progressively losing the Icelandic freshwater habitat signal, and becoming clearly restricted to marine habitats in winter. Some individuals begin to move locally to freshwater habitats, joining CBTG in a stopover at the end of the wintering period in preparation for northward migration.     

Influence of ultrasound on extraction of tannins from deoiled salseed cake

Deoiled salseed cake which contains 13–18% of tannins has extensive use in the production of poultry and cattle feed mixtures, where the tannin content is reduced to 4% or less. Studies have been carried out to remove tannins by the application of ultrasound as a function of frequency (43, 720 and 1000 kHz); intensity (2 to 9 W cm^?2); time (0 to 60 min); and by using different solvents. It has been observed that the percentage of extraction is greater at lower frequencies: 78% of tannins is extracted in a 40% aqueous acetone solvent using ultrasound in only 30 min compared to 20 h with conventional techniques.     

Magnetic solid‐phase extraction based on carbon nanotubes for the determination of polyether antibiotic and s‐triazine drug residues in animal food with LC–MS/MS

Carbon nanotubes‐magnetic nanoparticles, comprising ferroferric oxide nanoparticles and carbon nanotubes, were prepared through a simple one‐step synthesis method and subsequently applied to magnetic solid‐phase extraction for the determination of polyether antibiotic and s‐triazine drug residues in animal food coupled with liquid chromatography with tandem mass spectrometry. The nanocomposites were characterized by transmission electron microscopy, X‐ray diffraction, and vibrating sample magnetometry. The components within the nanocomposites endowed the material with high extraction performance and manipulative convenience. Compared with carbon nanotubes, the as‐prepared carbon nanotubes‐magnetic nanoparticles showed better extraction and separation efficiencies for polyether antibiotics and s‐triazine drugs thanks to the contribution of the iron‐containing magnetic nanoparticles. Various experimental parameters affecting the extraction efficiency had been investigated in detail. Under the optimal conditions, the good linearity ranging from 1 to 200 μg/kg for diclazuril, toltrazuril, toltrazuril sulfone, lasalocid, monensin, salinomycin, narasin, nanchangmycin, and maduramicin, low limits of detection ranging from 1 to 5 μg/kg, and satisfactory spiked recoveries (77.1–91.2%, with the inter relative standard deviation values from 4.0 to 12.2%) were shown. It was confirmed that this novel method was an efficient pretreatment and enrichment procedure and could be successfully applied for extraction and determination of polyether and s‐triazine drug residues in complex matrices.     

畜禽肉及饲料中氟苯尼考残留免疫分析方法研究

针对动物源性食品及饲料中氟苯尼考的残留问题,通过抗原制备、动物免疫和细胞融合筛选,成功得到可高特异性识别氟苯尼考的单克隆抗体,并建立了氟苯尼考的间接竞争酶联免疫分析（icELISA）方法。经单因素实验优化策略,确定最佳反应条件为：包被抗原质量浓度0.05 μg/mL,抗体质量浓度为0.1 μg/mL,最佳药物、抗体和二抗稀释液均为磷酸缓冲液（PBST）,抗体稀释液吐温－20含量0.05%,竞争反应时间30 min,二抗质量浓度为0.167 μg/mL,二抗反应时间30 min。在该条件下,建立了氟苯尼考的icELISA 检测方法,其IC50为9.48 ng/mL,线性检测范围为1.75 ~ 51.36 ng/mL,检出限（LOD）达0.64 ng/mL,且与氯霉素等结构及功能类似物均无明显交叉反应,特异性良好。实际样品的加标回收率为88.1% ~ 107%,相对标准偏差（RSD）< 15%。将所建立的方法用于畜禽肉及饲料样品的检测,结果与HPLC－MS/MS判定结果一致,说明该方法适用于畜禽产品及饲料中氟苯尼考的残留检测。     

QuEChERS-同位素稀释-气相色谱-串联质谱法测定动物源性食品中9种N-亚硝胺类化合物

建立了同时测定动物源性食品中9种N-亚硝胺类化合物的气相色谱-串联质谱分析方法。当下动物源性食品中N-亚硝胺类化合物污染种类较多,对人体危害较大,但国标GB 5009.26-2016仅针对N-二甲基亚硝胺的检测,且存在样品前处理复杂、标准方法回收率低、再现性差等问题,因此建立同时快速检测多种N-亚硝胺类化合物的方法有一定现实意义。称取10.0 g样品,置于50 mL离心管中,加入200 μL内标工作液和10 mL乙腈,冷冻30 min后,加入4 g硫酸镁和1 g氯化钠进行脱水,以9000 r/min离心5 min。取5 mL上清液使用150 mg聚苯乙烯二乙烯苯(PLS-A)粉末净化,再使用1.6 g MgSO₄和0.4 g NaCl脱水,过0.22 μm滤膜,上机分析。在初始温度为50 ℃时采用程序升温模式,0.16 min后,以900 ℃/min的速率将温度升至220 ℃。采用毛细管气相色谱柱HP-Innowax(30 m×0.25 mm×0.25 μm)分离,使用电子轰击电离(EI)源检测,在多反应监测模式下,以保留时间和特征离子对信息进行定性和定量分析,使用内标法定量N-亚硝胺类化合物。结果表明,N-亚硝胺类化合物在0.1~50.0 μg/L范围内具有良好的线性关系,方法的检出限(S/N=3)和定量限(S/N=10)分别为0.03~0.30 μg/kg和0.10~1.00 μg/kg。对不同样品基质进行0.5、1.0、3.0 μg/kg3个水平的加标回收试验,9种N-亚硝胺类化合物的回收率为80.4%~98.5%, RSD(n=6)为2.41%~12.50%。应用建立的方法检测市面上常见的动物源性食品,除N-亚硝基乙胺、N-亚硝基吗啡胆碱外,其他7种N-亚硝胺类化合物均有不同程度检出。检测结果表明,腌制水产品中N-亚硝胺类化合物含量普遍高于其他样品。研究建立的方法操作简单,不需要长时间蒸馏提取,可快速对动物源性食品中N-亚硝胺类化合物进行定性和定量分析,且样品和试剂的消耗量更少,节省成本,对环境污染小。该法的建立对我国动物源性食品中N-亚硝胺类化合物残留水平的控制、检测标准的制定和采取相应的管理措施具有一定的理论和现实意义。     

Ezetimibe-Loaded Nanostructured Lipid Carrier Based Formulation Ameliorates Hyperlipidaemia in an Experimental Model of High Fat Diet

Ezetimibe (EZE) possesses low aqueous solubility and poor bioavailability and in addition, its extensive hepatic metabolism supports the notion of developing a novel carrier system for EZE. Ezetimibe was encapsulated into nanostructured lipid carriers (EZE-NLCs) via a high pressure homogenization technique (HPH). A three factor, two level (2³) full factorial design was employed to study the effect of amount of poloxamer 188 (X1), pressure of HPH (X2) and number of HPH cycle (X3) on dependent variables. Particle size, polydispersity index (PDI), % entrapment efficiency (%EE), zeta potential, drug content and in-vitro drug release were evaluated. The optimized formulation displays pragmatic inferences associated with particle size of 134.5 nm; polydispersity index (PDI) of 0.244 ± 0.03; zeta potential of −28.1 ± 0.3 mV; % EE of 91.32 ± 1.8% and % CDR at 24-h of 97.11%. No interaction was observed after X-ray diffraction (XRD) and differential scanning calorimetry (DSC) studies. EZE-NLCs (6 mg/kg/day p.o.) were evaluated in the high fat diet fed rats induced hyperlipidemia in comparison with EZE (10 mg/kg/day p.o.). Triglyceride, HDL-c, LDL-c and cholesterol were significantly normalized and histopathological evaluation showed normal structure and architecture of the hepatocytes. The results demonstrated the superiority of EZE-NLCs in regard to bioavailability enhancement, dose reduction and dose-dependent side effects.     

Phytochemical Profile and Antioxidant Activities of Coleus amboinicus Lour. Cultivated in Indonesia and Poland

Coleus amboinicus Lour., Lamiaceae, is a perennial herb that is native to Indonesia and also cultivated in Africa, Asia and Australia. The major phytochemicals responsible for its bioactivity are rosmarinic acid (RA) and its analogues, flavonoids and abietane diterpenoids. The possibility of cultivation in a colder climate would extend the use of this herb and provide new opportunities to herb growers and livestock farmers. Our study to compare feed value and phytochemical composition of C. amboinicus plants cultivated in its original region, Indonesia, and in Poland. The crude protein content was significantly higher in plants cultivated in Indonesia compared to those cultivated in Poland—21% and 13% of dry matter, respectively. The higher ADF contents were detected in C. amboinicus cultivated in Indonesia, 38–41%, in comparison to 34% in plants cultivated in Poland. The phytochemical composition was also significantly influenced by the cultivation location. Polish samples were higher in polyphenols (RA and its analogues), and also had 1.5–2-fold higher antioxidant potential, as measured by DPPH scavenging, phosphomolybdenum reduction and Fenton reaction driven lipid peroxidation. The Indonesian samples contained more diterpenoid compounds, such as dihydroxyroyleanone, and the sum of terpenoids was ca. 10 times higher than in samples from Poland (15.59–23.64 vs. 1.87 µg/g of extracts). In conclusion, C. amboinicus is suitable for cultivation in non-optimal climatic conditions but some nutritional properties and bioactivity are significantly affected.     

探讨妊娠糖尿病运用个体化营养膳食的影响

目的了解妊娠期糖尿病专业治疗中行个体化营养膳食疗法对其妊娠结局以及血糖控制水平产生的影响。方法选择130例因妊娠期糖尿病进入江西省萍乡市人民医院的患者,以膳食疗法的差异分组:62例Ⅰ组施以常规膳食疗法,68例Ⅱ组则施以个体化营养膳食疗法,再对两组病例血糖值及其妊娠结局专业统计、观察。结果施以两种膳食疗法后,62例Ⅰ组FPG值(5.60±0.90)mmol/L,68例Ⅱ组(4.47±0.49)mmol/L,(P<0.05);同时Ⅱ组2h PG值及其妊娠结局等都优于Ⅰ组,(P<0.05)。结论对于患有糖尿病的妊娠期患者,通过施以个体化营养膳食疗法,可实现对妊娠结局的充分改善,值得推荐应用。     

Effects of Wine Components in Inflammatory Bowel Diseases

With the rising prevalence of Inflammatory bowel disease (IBD) worldwide, and the rising cost of treatment with novel biological drugs, there is an increasing interest in various diets and natural foods as a potential way to control/modulate IBD. As recent data indicates that diet can modify the metabolic responses essential for the resolution of inflammation, and as wine compounds have been shown to provide substantial anti-inflammatory effect, in this review we aimed to discuss the current evidence concerning the impact of biological compounds present in wine on IBD. A number of preclinical studies brought forth strong evidence on the mechanisms by which molecules in wine, such as resveratrol or piceatannol, provide their anti-inflammatory, anti-oxidative, anti-tumor, and microbiota-modulation effects. However, concerning the effects of alcohol, it is still unclear how the amount of ethanol ingested within the framework of moderate wine consumption (1–2 glasses a day) affects patients with IBD, as human studies regarding the effects of wine on patients with IBD are scarce. Nevertheless, available evidence justifies the conductance of large-scale RCT trials on human subjects that will finally elucidate whether wine can offer real benefits to the IBD population.