Natural estrogens in dairy products: Determination of free and conjugated forms by ultra high performance liquid chromatography with tandem mass spectrometry

Natural estrogens are synthesized by mammals in different amounts depending on the developmental stage and pregnancy/lactation period, and they may pass into milk, where they are mostly present as glucuronated and sulfated forms. In modern dairy practices, about 75% of milk is produced from pregnant cows; therefore, the amount of hormones that may pass into milk could be of concern. While estrogen determination in milk has been investigated in depth, the individual determination of estrogens and their conjugated forms in dairy products has not been fully addressed. The aim of this work was to develop and assess a sensitive method, using the peculiar retention properties of graphitized carbon black, to extract natural free estrogens and their major conjugated metabolites, without any enzymatic cleavage, from yogurt, cheese, and butter. The free and conjugated estrogens were eluted in two distinct fractions from the solid‐phase extraction cartridge and analyzed separately by ultra high performance liquid chromatography coupled to tandem mass spectrometry. Recoveries were higher than 80% for all the three sample typologies. The highest matrix effects were observed for butter, which was richest in lipid content, but was below 30%. A survey on some commercial dairy products suggests that production processes decreased estrogen content.     

浊点萃取-荧光光度法测定水中的苯酚

基于非离子表面活性剂Triton X-100,以浊点萃取结合荧光光度法测定水中的苯酚,考察影响浊点萃取的各种因素。在pH=3.0的磷酸氢二钠-磷酸二氢钾缓冲溶液中,采用2.0mL Triton X-100(5%)、82℃平衡温度、8min平衡时间的条件下,苯酚被萃取到Triton X-100表面活性剂相与水相分开,用于环境水样中苯酚的测定,结果令人满意。     

全自动凝胶净化-浓缩-固相萃取/气相色谱-质谱法测定紫皮石斛中有机磷农药残留

建立了以凝胶渗透色谱(GPC)和固相萃取(SPE)净化、气相色谱-质谱(GC-MS)法同时测定紫皮石斛中10种有机磷农药残留的方法。样品用乙腈超声提取,提取液经GPC去除类脂杂质和大分子物质,后经Envi-Carb/NH2固相萃取柱净化,选择离子(SIM)监测模式检测,外标法定量。在26min内10种农药得到很好的分离,农药残留量在0.02~0.5μg/mL,方法的线性良好,相关系数为0.997 3~0.999 9,农药加标浓度为0.05mg/kg和0.2mg/kg时,加标回收率在70.4%~115.8%,相对标准偏差在2.8%~9.6%,满足国家标准要求,检出限为0.005 2~0.011mg/kg。方法简便、快速、灵敏、准确,能够运用于石斛中多组分有机磷农药残留的定性和定量分析。     

Ultrasound-assisted green extraction methods: An approach for cosmeceutical compounds isolation from Macadamia integrifolia pericarp

This study aimed was to examine the potential of several green extraction methods to extract cosmetic/cosmeceutical components from Macadamia integrifolia pericarps, which were a by-product of the macadamia nut industry. M. integrifolia pericarps were extracted by conventional solvent extraction process using 95% v/v ethanol and various green extraction methods, including infusion, ultrasound, micellar, microwave, and pulsed electric field extraction using water as a clean and green solvent. The extracts were evaluated for total phenolic content using Folin-Ciocalteu method. The antioxidant activities were evaluated by 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2′-azinobis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), ferric reducing/antioxidant power, and ferric-thiocyanate method. The anti-skin ageing activities were investigated by means of collagenase, elastase, and hyaluronidase inhibition using enzyme-substrate reaction assay. The irritation profile of the extracts was evaluated by the hen’s egg test-chorioallantoic membrane (HET-CAM) test. The results noted that ultrasound-assisted extraction yielded the significantly highest extract amount with the significantly highest total phenolic content (p < 0.05), especially when the extraction time was 10 min. The aqueous extract from ultrasound-assisted extraction possessed the most potent antioxidant and anti-skin ageing activities (p < 0.05). Its antioxidant activities were comparable to ascorbic acid and Trolox, whereas the anti-skin ageing activities were equivalent to epigallocatechin-3-gallate and oleanolic acid. Besides, the extract was safe since it induced no irritation in the HET-CAM test. Therefore, ultrasound-assisted extraction was suggested as an environmentally friendly extraction method for M. integrifolia pericarp extraction and further application in the cosmetic/cosmeceutical industries.     

Modifications to functional and biological properties of proteins of cowpea pulse crop by ultrasound-assisted extraction

Natural resource depletion, negative environmental effects and the challenge to secure global food security led to the establishment of the Sustainable Development Goals (SDGs). In need to explore underutilized sustainable protein sources, this study aims at isolating protein from cowpea by ultrasound-assisted extraction (UAE), where the techno-functional characteristics of the protein isolates were studied at different sonication conditions i.e., 100 W and 200 W at processing times ranging from 5 to 20 min. The US at 200 W-10 min produced the optimal results for all properties. In this process combination, there was an increase in protein yield, solubility, water-holding capacity, foaming capacity and stability, emulsion activity and stability, zeta-potential, and in-vitro protein digestibility from 31.78% to 58.96%, 57.26% to 68.85%, 3.06 g/g to 3.68 g/g 70.64% to 83.74%, 30.76% to 60.01%, 47.48% to 64.26%, 56.59% to 87.71%, –32.9 mV to −44.2 mV and 88.27% to 89.99%, respectively and particle size dropped from 763 nm to 559 nm in comparison to control. The microstructure and secondary-structure alterations of proteins caused by sonication were validated by SEM images, SDS-PAGE, and FTIR analyses. Sonication leads to acoustic cavitation and penetrate the cell walls, improving extraction from the solid to liquid phase. After sonication, the hydrophobic protein groups were exposed and proteins were partially denatured which increased its functionality. The findings demonstrated that UAE of cowpea protein improved yield, modify characteristics to fit the needs of the food industry, and contribute to achieving SDGs 2, 3, 7, 12, and 13.     

Ultrasound-assisted extraction,analysis and antioxidant activity of polysaccharide from the rinds of Garcinia mangostana L.

According to response surface methodology (RSM), the extraction conditions of ultrasound-assisted extraction of polysaccharide from the rinds of Garcinia mangostana L. (GMRP) were optimized and determined. The optimal conditions obtained through optimization were: the liquid to material ratio was 40 mL/g, ultrasonic power was 288 W and extraction time was 65 min. The average extraction rate of GMRP was 14.73%. Ac - GMRP was obtained by acetylation of GMRP, and the antioxidant activities of the two polysaccharides were compared in vitro. The results indicated that the antioxidant capacity of polysaccharide obtained after acetylation was significantly improved compared with that of GMRP. In conclusion, chemical modification of polysaccharide is an effective measure to improve its properties to a certain extent. Meanwhile, it implies that GMRP has great research value and potential.     

Ultrasound-assisted extraction and analysis of maidenhairtree polysaccharides

The maidenhairtree polysaccharides (MTPs) have important application prospects. So, the extraction, purification, structure, derivatization and biological activities of polysaccharides from leaves, fruits, and testae of maidenhairtree were disscussed. Polysaccharides were extracted by collaborative extraction methods such as ultrasound-assisted extraction and microwave-assisted extraction. The ultrasound-assisted extraction had higher content and higher efficiency. The structural characteristics and structure-activity relationship of maidenhairtree polysaccharides were studied in order to provide theoretical basis and technical support for the further development and utilization of maidenhairtree polysaccharides.     

“海水提镁”项目式教学设计与实践*

依托广西北海市丰富的海洋资源,创设了“在北海能否建提镁厂”的驱动性总任务,师生合议将任务规划为3个大问题和6个子任务。学生采用信息收集、分类、比较、推理、实验、系统分析等认知策略,最终以ppt的形式进行成果汇报,通过组间评价、核心问题讨论、决策性问题辩论等方式逐步落实项目目标。     

Polyimidazolyl acetate ionic liquid grafted on cellulose filter paper as thin-film extraction phase for extraction of non-steroidal anti-inflammatory drugs from water

Recently, pharmaceuticals and personal care products in the water environment exhibited potential risks to both human and aquatic organisms. In order to improve the sensitivity and accuracy of pharmaceutical detection, the polyimidazolyl acetate ionic liquid was synthesized by Radziszewski reaction and coated on cellulose filter papers as a thin-film extraction phase for extraction of non-steroidal anti-inflammatory drugs from water. The attenuated total reflection-infrared spectrometry, thermogravimetric analysis, and scanning electron microscope analyses demonstrated that the polyimidazolyl acetate ionic liquid was successfully prepared and attached to the surface of the cellulose filter paper through chemical bonding. The adsorption capacity of the homemade thin-film extraction material for the four non-steroidal anti-inflammatory drugs was greater than 8898 ng/cm² under the optimum conditions, and the desorption rate was over 90%. Then, a paper-based thin-film extraction phase-high-performance liquid chromatography-tandem mass spectrometry method was established for the extraction of non-steroidal anti-inflammatory drugs in water. This method provided limits of detection and limits of quantification were in the range of 0.02–0.15 and 0.17–0.50 μg/L, respectively. Hence, the obtained thin-film extraction phase showed excellent recovery and reproducibility for the target non-steroidal anti-inflammatory drugs with carboxyl groups from water.     

Facile synthesis of a novel magnetic covalent organic frameworks for extraction and determination of five fungicides in Chinese herbal medicines

A novel magnetic covalent organic framework was synthesized via a one-step coating approach with solvothermal reaction employing 2,4,6-tris(4-aminophen-yl)-1,3,5-triazine and 2,4,6-triformylphloroglucinol as two building blocks by covalent bonding. The prepared magnetic covalent organic frameworks were properly characterized by different techniques and employed as adsorbents of magnetic solid-phase extraction. An analytical method was developed for the simultaneous determination of five fungicides in two Chinese herbal medicine samples via magnetic solid-phase extraction coupled to ultra high performance liquid chromatography with tandem mass spectrometry analysis. Under optimized magnetic solid-phase extraction conditions, the method exhibited satisfactory recoveries (74.0−109.6%) with relative standard deviations of 0.4−4.6%, low limits of detection (0.003−0.015 μg/kg), and good linearity (R² > 0.9960). Compared with the traditional extraction method, the proposed method required a lower amount of adsorbent (3 mg) and extraction time (5 min). The adsorbent also had favorable reusability (not less than eight times). Therefore, the magnetic covalent organic frameworks could be a promising adsorbent for the extraction and quantitation of fungicides in Chinese herbal medicines.