A reliable and sensitive time-resolved fluorescent immunochromatographic assay (TRFICA) for ochratoxin A in agro-products

Immunochromatographic assays (ICAs) are considered as a suitable diagnostic tool for the detection of mycotoxins. Mycotoxins and especially, ochratoxin A are analytes with more demanding sensitivity requirements. To enhance the sensitivity of current immunochromatographic assays for ochratoxin A (OTA), a novel sensitive ICA was developed in this study. In the assay, microspheres enclosing fluorescent europium (III) [Eu(III)] nanoparticles (EuNPs) were used as a label for OTA monoclonal antibody (OTA-mAb) conjugation. Accordingly, assay was called time-resolved fluorescent immunochromatographic assay (TRFICA). The test strip was composed of three parts: a sample pad, nitrocellulose membrane and an absorbent pad. As for detection, a proper concentration of conjugated microspheres was pipetted into the microtube and sample extract was added to it. Then the strip was inserted into the tube and the fluid flow along the strip. The TRFICA results were obtained in 8 min and read by a portable TRFICA strip reader. The established method allows quantitative determination of OTA with limit of detection as low as 1.0 μg kg⁻¹ in the samples. For validation, spiked samples including wheat, maize, soybean and rice were respectively assayed by TRFICA and a standard high performance liquid chromatography equipped with a fluorescence detector (HPLC-FLD), and good agreement of results was obtained between two methods.     

Rapid detection method for aflatoxin B1 in soybean sauce based on fluorescent microspheres probe

Soybean sauce, a Chinese traditional and daily condiment, is often contaminated by aflatoxin B₁. An extract-free immunochromatographic assay was proposed based on fluorescent microspheres probe for the' detection of aflatoxin B₁ in soybean sauce. The probe was prepared by coupling fluorescent microspheres with anti-aflatoxin B₁ antibody by the 1-ethyl-3(3-dimethylaminopropyl) carbodiimides hydrochloride-mediated method. The background from the soybean sauce sample on strip was eliminated because of the optical property of the probe. The sample without extracting procedure was directly detected by diluting with 10% methanol solution. The visible detection limit for the qualitative analysis of aflatoxin B₁ in the proposed method was 2.5 μg/L, which was lower than the maximum level of 5 μg/L set by the Chinese government. The results were well agreed with those obtained by liquid chromatography-mass spectrometry (LC-MS). The method showed satisfactory characteristics, such as rapid detection, easy operation, and high sensitivity, and can thus be applied for the large-scale and on-site screening of soybean sauce contaminated with aflatoxin B₁. To our knowledge, this report is the first one on the qualitative detection of aflatoxin B₁ in dark colored food samples directly by fluorescent microspheres probe-based immunochromatography.     

Influence of ultrasonic treatment on the structure and emulsifying properties of peanut protein isolate

Effects of ultrasonic treatment on emulsifying properties and structure of peanut protein isolate (PPI) were evaluated by analysis of particle size distribution, protein surface hydrophobicity, SDS-PAGE, circular dichroism spectra and environmental scanning electron microscopy. The emulsifying properties of the PPI were found to be improved by ultrasonic treatment. The mean particle size decreased from 474.7 nm to 255.8 nm while the molecular weight remained unaffected. The results of intrinsic fluorescence spectroscopy and surface hydrophobicity indicated that ultrasonic treatment induced tertiary structural changes of the proteins in PPI. Emulsifying activity index and emulsion stability index were found to be correlated fairly well with surface hydrophobicity (H₀) (r = 0.712 and r = 0.668, respectively).     

抗衰老保健食品中白藜芦醇和辅酶Q10的含量测定

建立了同时测定抗衰老保健食品中白藜芦醇和辅酶Q10的含量的HPLC方法。采用Welch materials C18液相色谱柱,甲醇∶异丙醇(55∶45)为流动相,流速设定为1 mL·min-1,检测波长为PDA定时波长(0.00,306.0)(6.00,306.0)(6.01,275.0)(20.00,275.0),实现了白藜芦醇和辅酶Q10的良好分离分析。白藜芦醇的线性范围为0.52～156.00μg·mL-1,r=0.9999;辅酶Q10的线性范围为0.49～195.52μg.mL-1,r=0.9999。平均加标回收率及RSD分别为97.70%(RSD 0.6%)和97.40%(RSD 0.4%)。本方法灵敏度高、选择性好、操作简单,可方便地用于检测抗衰老类保健食品中白藜芦醇和辅酶Q10的含量。     

水相中酒石酸铀酰形态的电喷雾串联质谱研究

铀的水溶液化学形态是高放废物处置研究的重要内容之一。本实验采用电喷雾串联质谱（ESI-MS/MS）研究酒石酸-硝酸铀酰水溶液中铀酰形态,共分析出14种酒石酸铀酰和5种无机铀酰形态。每个铀酰基团可紧密结合1个酒石酸阴离子,并继续以较弱的形式络合1~2个酒石酸分子。实验中还发现了［(UO₂HTarH₂Tar)₂］²⁺、［(UO₂)₃Tar(HTar)₂(H₂Tar)₂］²⁺等酒石酸铀酰团簇形态。酒石酸铀酰形态中各络合键解离所需能量大小顺序为：铀酰间结合键＞酒石酸阴离子-铀酰结合键＞酒石酸分子-铀酰结合键。该研究对实际条件下铀与有机酸的水溶液形态研究具有指导意义。     

基于雷达图与紫外-可见分光光度法建立鱼汤挥发性风味评价方法及其应用

目的建立感官评价与浓度评价相结合的鱼汤挥发性风味综合评价斱法,幵应用于鱼汤配料配斱研究。方法应用感官评分表、雷达图及紫外-可见分光光度法(ultraviolet-visible spectrophotometry, UV-Vis)等可视化手段将感官评价与浓度评价结合建立鱼汤挥发性风味评价斱法,其中感官评价从鱼腥味、油脂香、豆腥味、生姜味、大蒜味、清香、综合7个感官剖面开展幵应用雷达图分析,浓度评价以风味萃取物的UV-Vis吸收值考察。结果基于所建立的评价斱法,鱼肉250 g,大豆油、生姜、大蒜添加量为鱼肉重的9%、1.2%、3.5%时,所制作的鱼汤风味最佳。结论本研究建立的斱法直观、快捷、简单,可操作性强,兊服了单一感官或浓度评价的不足,可拓展应用于新产品开发或新工艺的研究。     

固相萃取-超高效液相色谱-三重四极杆质谱法测定甘蔗中3-硝基丙酸

目的建立固相萃取-超高效液相色谱-三重四极杆质谱联用技术(solidphaseextraction-ultra performanceliquidchromatographytandemmassspectrometry,SPE-UPLC-MS/MS)测定甘蔗中3-硝基丙酸(3-nitropropionic acid, 3-NPA)的分析方法。方法甘蔗汁和甘蔗渣经PSA固相萃取提取净化,以1%氨水甲醇溶液洗脱,氮吹吹干定容于0.5%甲酸水溶液中,以Waters HSS T3色谱柱(2.1 mm×50 mm, 1.8μm)在流动相乙腈-水(1:1,V:V)条件下进行分离,电喷雾负离子MRM模式下检测,以基质标准曲线定量。结果甘蔗汁中3-硝基丙酸的线性范围为5～1000μg/kg,检出限(S/N=3)为1.2μg/kg,甘蔗渣中线性范围为10～1000μg/kg,检出限(S/N=3)为2.7μg/kg。甘蔗汁和甘蔗渣3-NPA的加标回收率为96.5%～101.2%,相对标准偏差为1.54%～5.35%。结论该方法简单、灵敏、准确,可用于甘蔗中3-硝基丙酸检测。     

电感耦合等离子体质谱法测定食品接触材料及制品中钡、钴、铜、铁、锂、锰的迁移量

目的建立电感耦合等离子体质谱法同时测定食品接触材料及制品中钡、钴、铜、铁、锂、锰元素含量的方法。方法采用水、4%乙酸、10%乙醇、20%乙醇、50%乙醇和95%乙醇(V:V)作为食品模拟物进行迁移试验,试样溶液根据基质的差异选择不同的前处理方式,优化仪器参数和实验条件,最后由电感耦合等离子体质谱仪同时测定迁移试样溶液中6种金属元素的含量。结果各金属元素在一定的浓度范围内线性关系良好,相关系数大于0.999,方法检出限为0.3～9.0μg/kg,样品平均加标回收率为86.5%～109.1%,相对标准偏差为1.0%～8.3%。结论该方法简便易于操作,稳定可靠,检出限低,完全能够满足GB 9685-2016《食品安全国家标准食品接触材料及制品用添加剂使用标准》对金属元素特别限制规定的检测需求,为食品接触材料及制品中多种金属元素迁移量提供了一种高效可行的检测手段。     

SPME-GC-MS法分析草鱼汤烹制过程中挥发性成分变化

采用固相微萃取和气相色谱-质谱联用技术,研究传统鱼汤烹制过程中挥发性成分的变化。草鱼肉块经油煎后与生姜、大蒜混合水煮制作鱼汤,煮制分为3 个时间段,0～10 min鉴定出挥发性化合物46 种,其中萜类20 种、芳香族9 种、醛类5 种、酮类2 种、醇类3 种、呋喃类3 种、含硫化合物3 种、其他1 种;11～20 min鉴定出挥发性化合物43 种,其中萜类22 种、芳香族3 种、醛类4 种、酮类1 种、醇类5 种、呋喃类2 种、含硫化合物4 种、其他2 种;21～30 min鉴定出挥发性化合物53 种,其中萜类21 种、芳香族5 种、醛类11 种、酮类3 种、醇类5 种、呋喃类2 种、含硫化合物3 种、其他3 种。这些化合物当中,萜和含硫化合物来源于生姜和大蒜,主要形成于煮制的初始阶段且含量在煮制过程中不断下降;醛、醇、酮等化合物主要由脂肪酸氧化形成,且在煮制过程中种类不断丰富,含量逐渐增加。油煎和调料添加是鱼汤风味化合物形成的主要原因,煮制是挥发性风味化合物种类不断丰富和含量平衡的过程。