水产品及养殖水中丁香酚类化合物风险研究

目的 检测水产品及养殖水中丁香酚类化合物。方法 应用食品补充检验方法BJS 201908《水产品及水中丁香酚类化合物的测定》，以海水鱼、淡水鱼、海水虾、淡水虾及养殖水作为基质，测定6种丁香酚类化合物的含量。结果 通过对实际样品测定后发现，在水产品中检出了丁香酚类化合物，主要为丁香酚，检出率为28.9%，其中海水鱼相对突出。结论 本研究为丁香酚作为渔用麻醉剂提供了方法论，为丁香酚类化合物在水产运输的合理使用提供理论依据。     

Environmental impact estimation of ceramic lightweight aggregates production starting from residues

Within a circular economy approach, this study investigates the environmental impact of lightweight aggregates (LWAs) produced starting from different mixes of different clays with brewery sludge and cattle bone flour ash (CBA), used as poring and fertilizing agents, respectively. The environmental impact was evaluated by means of release tests, insulation capacity, carbon footprint (CFP), and particulate matter emission during pellet firing. Release tests representative of LWAs realistic application showed very high release of phosphate and satisfactory release of potassium. The thermal insulation of the LWAs was tested by thermal imaging camera and resulted highly variable depending on the composition, with the mix containing CBA performing best. This latter composition leads also to the smallest CO₂ equivalent emission, due to the calorific power of CBA, allowing lower consumption of fossil fuels during the LWA production. Finally, total particulate emissions during the thermal treatment resulted similar in terms of mass for all mixes, while differences in terms of particle morphology and composition occurred. Samples containing residue resulted with a quite good release behavior, CFP, and insulation properties, but higher emission of particles, particularly when glass is added.     

QuECHERS-超高效液相色谱-串联质谱法快速检测阿克苏红枣中29种农药残留量

目的 建立QuECHERS-超高效液相色谱-串联质谱法快速检测红枣中29种农药残留量。方法 样品用0.1%乙酸-乙腈溶液振荡提取, QuECHERS净化, 以waters BEH C18色谱柱分离, 在正离子模式下选用多反应监测模式进行检测, 外标法定量。结果 29种农药在0.005~0.2 mg/L线性关系良好, 相关系数大于0.995, 加标浓度为10、50、100 μg/kg时, 平均回收率为74.6%~109.1%, 相对标准偏差均<15%, 检出限为0.15~ 3.0 μg/kg。结论 该方法操作简便, 准确可靠, 稳定性强, 适用于红枣中29种农药残留量的快速测定。     

加速溶剂萃取-气相色谱-串联质谱法测定菊花中多种农药残留

目的建立一种加速溶剂萃取结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时检测菊花中123种农药残留的方法。方法样品采用乙腈提取,经加速溶剂萃取,石墨化碳/氨基固相萃取小柱净化,SH-Rxi-5SilMS (30 m×0.25 mm, 0.25μm)毛细管色谱柱分离,在气相色谱串联质谱多反应监测离子(multiple reaction monitoring, MRM)扫描模式下进行测定,基质外标法定量。结果在0.005～0.5mg/L范围内,123种农药有良好的线性关系(r~2≥0.9967),方法检出限为0.5～29.1μg/kg,定量下限为1.7～97.1μg/kg,在100、200、400μg/kg 3个添加水平下,123种农药的平均回收率在70.0%～128.8%之间,相对标准偏差(RSD)在0.5%～10.1%。结论该方法提取效率高、准确、灵敏,可应用于菊花中多种农药残留的筛查与测定。     

气相色谱-串联质谱法测定植物性食品中50种农药残留

目的建立QuEChERS前处理、气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)结合基质匹配标准系列测定植物性食品中50种农药的分析方法。方法样品经乙腈提取,QuEChERS净化,采用正构烷烃保留指数法确定待测农药保留时间,最后经三重四极杆质谱仪结合基质匹配标准系列定性及定量检测。结果在0.05～2.00μg/mL范围内50种农药线性良好,相关系数r均大于0.995,方法检出限在0.002～0.007 mg/kg,加标回收率为77.7%～122%,相对标准偏差(relative standard deviation, RSD)为1.9%～12.1%。结论本方法具有简便、快速、检测结果较准确的特点,适合测定植物性食品中50种农药残留。     

高效液相色谱-串联质谱法测定能力验证肉粉中四环素类抗生素残留量

目的优化肉粉样品中四环素类药物的高效液相色谱-串联质谱检测方法。方法采用80%乙腈-水溶液提取肉粉样品中的四环素类药物,Prime HLB固相萃取小柱净化,洗脱液用氮气吹至近干,用10%乙腈水溶液(含0.2%甲酸)溶解,采用多反应监测正离子模式(multiple reaction monitoring, MRM)进行高效液相色谱-串联质谱仪测定。结果与国标方法GB/T 21317-2007(HLB固相小柱萃取法)相比,4种药物的线性范围均在5～200μg/L时线性良好(r 0.99),回收率差异不显著(P0.05)。实验室方法测得的含量分别为:四环素113.93μg/kg,金霉素68.16μg/kg,多西环素155.73μg/kg,土霉素未检出;回收率为四环素94.5%,金霉素95.2%,多西环素104.7%,土霉素97.8%。测得四环素、金霉素、多西环素、土霉素线性相关系数r分别为:0.9995、0.9998、0.9989、0.9997。结论本实验室方法简单快速,回收率高,重现性好,适用于熟肉制品中四环素类药物的多残留检测。     

QuEChERS结合GC-MS/MS法测定果蔬汁中21种农药残留

建立一种采用QuEChERS前处理结合Quick Pro净化柱-气相色谱串联质谱（GC-MS/MS）法测定果蔬汁中的21种农药残留量的方法。样品采用乙腈提取，EN方法盐包盐析，经Quick Pro净化柱净化，DB-35MS UI色谱柱分离，采用选择离子监测（SIM）模式扫描，外标法定量。在质量浓度0.01～0.50 μg/mL范围内相关系数（R）均＞0.995，样品在0.01 mg/kg、0.02 mg/kg、0.10 mg/kg的添加水平下，21种农药的回收率在75.2%～117.8%之间，回收率实验结果相对标准偏差（RSD）在1.9%～11.5%之间。该方法操作简便，分析时间短，精密度好，适用于果蔬汁中多种农药残留的检测。     

聚碳酸酯水桶中5种酚类物质的残留量检测以及迁移风险评估

目的利用超高效液相色谱法研究聚碳酸酯水桶(polycarbonate, PC)中5种酚类物质(苯酚、双酚A、对叔丁基苯酚、对枯基苯酚和2,4-二叔丁基苯酚)的残留量并对迁移风险进行评估。方法利用溶解-沉淀法对30批PC水桶中的酚类物质进行提取。参考GB 31604.1-2016《食品安全国家标准食品接触材料及制品迁移试验通则》和GB 5009.156-2015《食品安全国家标准食品接触材料及制品迁移试验预处理方法通则》对PC水桶进行迁移试验。利用超高效液相色谱法对提取液和迁移试液中的酚类物质进行定性和定量分析。结果在线性范围0.02～5mg/L内,线性系数均大于0.999,加标回收率在82%～109%之间,相对标准偏差范围为0.6%～5.2%(n=3)。30批饮用水桶中,各酚类物质的检出率分别为73%、93%、50%、43%和93%。食品模拟物为水的迁移实验中,只有苯酚和双酚A有检出,且数值都小于国家标准中的限量值。结论 5种酚类物质在PC水桶中的迁移风险都较小,研究可为PC产品的质量控制和酚类物质风险监测提供技术基础。     

果蔬汁中氯氰菊酯、多效唑、哒螨灵含量测定能力验证结果分析

目的分析果蔬汁中氯氰菊酯、多效唑、哒螨灵含量测定能力验证结果。方法本实验室参加中国检验检疫科学研究院测试评价中心组织的果蔬汁中氯氰菊酯、多效唑、哒螨灵的测定能力验证(ACAS-PT806-2019),根据能力验证作业指导书要求和样品情况,采用了QuEChERS样品前处理净化方案,气相色谱电子捕获检测器检测氯氰菊酯,内标法定量,液相色谱串联质谱检测多效唑和哒螨灵,外标法定量。结果 1号样品中氯氰菊酯、多效唑、哒螨灵残留量分别为0.098、0.043、0.084 mg/kg, 2号样品中氯氰菊酯、多效唑、哒螨灵残留量分别为:0.036、未检出、0.013 mg/kg。所有测定项目结果均为满意(|Z|≤2)。结论实验室解决了此次能力验证中没有空白样品,检测项目基质效应差异明显等难点。实验室农药残留检测能力得到有效验证和提高。     

The circular economy of agro and post-consumer residues as raw materials for sustainable ceramics

The circular economy in the area of waste management implies their re-use as a raw material in different production cycles. Both the qualitative and quantitative characteristics of the residues from the agro sector and those of the products of the ceramics sector make possible to think of a feasible application. This review will illustrate some examples of recycling of residues deriving from animal and vegetable sectors (and two post consume products, spent coffee grounds, and packaging glass cullet), studied by the authors, falling within the concept of urban and agricultural sustainable development. Not only the most traditional products such as glass-ceramics, glazes, bricks, but also the most innovative lightweight aggregates for plant structures or in and out soil cultivation, as well as additives such as deflocculants for ceramic suspensions, which will be illustrated from the design/production, characterization, and comparison with commercial products.