超高效液相色谱-高分辨质谱法快速筛查确证调味品中的19种非食用物质

目的建立超高效液相色谱-高分辨质谱法检测调味品中19种非食用物质的分析方法。方法样品经乙酸乙酯-环己烷提取,采用凝胶渗透色谱(gel permeation chromatography,GPC)净化与在线定量浓缩,然后经C_(18)色谱柱分离,乙腈和5 mmol/L乙酸铵(含0.1%甲酸)溶液梯度洗脱后经超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry,UPLC-LTQ-orbitrap MS)测定。结果 19种目标物在15 min内实现良好分离,线性相关系数均≥0.996,定量限(limit of quantitation,LOQ)为5~15μg/kg,加标回收率在61.9%~105.8%之间,相对标准偏差(relative standard deviation,RSD)为2.3%~12.9%。结论本研究建立的方法准确、简单,可适用于调味品中19种非食用物质的定性定量及确证分析。     

蜂蜜中元素含量检测的两种前处理方法比较

目的与传统的微波消解前处理方法比较,探索较优的前处理方法快速准确地检测蜂蜜中元素的含量。方法在GB 5009.268-2016《食品安全国家标准食品中多元素的测定》的基础上,基于蜂蜜基质的水溶性,对其前处理方法进行改进,优化。采用5 mL硝酸浸泡过夜,直接加二次水定容至50 mL,用电感耦合等离子体质谱仪进行检测。结果本方法测定蜂蜜中镁、钾、铜、锰元素含量与传统的微波消解前处理方法检测的含量无显著性差异。结论该方法准确、快速、简便,适用于大批量蜂蜜中镁、钾、铜、锰以及有毒有害元素含量的测定。     

RapidChek检测食品中单增李斯特菌的方法评价

目的评价RapidChek法检测食品中单增李斯特菌的检测效果并验证。方法采用t检验,比较RapidChek方法与GB 4789.30-2016方法的培养基增菌效果。依据ISO 16140:2003《食品和动物饲料微生物学-可替代方法的验证方案》,比较RapidChek检测方法与GB 4789.30-2016检测方法的检测效果,涉及的性能指标有相对准确性、相对特异性和相对灵敏度、包含性和排他性。结果 RapidChek检测方法增菌培养基效果优于GB 4789.30-2016方法增菌培养基LB_1。根据RapidChek检测方法、GB 4789.30-2016培养基+RapidChek试纸条方法、RapidChek培养基+GB 4789.30分离鉴定方法的统计检验得出,3种方法与参照方法在相对准确性、相对特异性和相对灵敏度方面无显著性差异。在包含性和排他性方面,RapidChek检测方法与GB 4789.30-2016检测方法的检测结果均一致。结论在所验证的指标上,RapidChek检测方法(包括与GB4789.30-2016组合的方法)与GB 4789.30-2016方法无差异。     

入境动物产品携带杂草疫情分析

系统分析2011~2015年山东口岸进境动物产品中杂草疫情的截获情况,旨在掌握进境动物产品中杂草截获的种类和规律,并有针对性地提出完善检疫监管措施的对策。共截获2407批次的杂草,其中检疫性杂草3科10属30种(属)52批次。按照来源国统计,从来自26个国家和地区的动物产品中截获杂草,其中以澳大利亚截获杂草批次和种次数最多,占到整个截获量的57.2%。根据以上情况分析,应加强进境动物产品中皮、毛的检疫力度。建议从风险评估、产地预检、检疫监管和处理、疫情监测、加强宣传沟通等多方面制定措施,建立外来杂草入侵防范体系,以有效防止外来有害杂草随寄主携带入侵我国。     

气相色谱- 串联质谱法测定食品中的富马酸二甲酯

为解决样品基体成分复杂、干扰测定的难题,建立一种基于气相色谱- 串联质谱(GC-MS/MS)检测食品中富马酸二甲酯的方法。通过对提取液、固相萃取柱、电离电压的考察,最终确定食品中富马酸二甲酯经乙腈提取、C18 小柱净化、CID 电压15V 最优条件。本方法在0.045～10.00mg/L 质量浓度范围内呈线性关系,相关系数为0.9998,仪器定量检出限LOQ 为0.045mg/L,外标法定量。在0.05、0.50、1.00mg/kg 3 个水平的回收相对标准偏差为2.77%～8.70%,回收率87%～108%。结果表明,相对于GC、GC-MS 方法,GC-MS/MS 方法分析时间短、无杂质峰干扰、灵敏度高,可以满足食品中检测的要求。     

纳米材料电化学传感器在食品安全检测中的应用

电化学传感器的发展已超过半个世纪, 纳米材料作为20世纪最伟大的发现之一, 目前已广泛应用于传感器领域。纳米材料电化学传感器具有灵敏度高、选择性好、操作简便、成本低等诸多优点,在分析领域有着广泛的应用。纳米材料电化学传感器在食品安全检测领域的应用研究正在蓬勃开展。本文综述了纳米材料电化学传感器在食品安全检测中的应用, 包括对化学残留和细菌的检测。     

凝胶渗透色谱净化-气相色谱-质谱法测定黄油中6种激素的残留

建立了凝胶渗透色谱(GPC)-气相色谱-质谱(GC/MS)同时测定黄油中雄酮(A)、脱氢表雄酮(DHEA)、睾酮(T)、孕酮(P)、雌酮(E1)、17β-雌二醇(β-E)6种类固醇激素残留的方法。黄油样品用乙酸乙酯/环己烷(1:1,V/V)振荡辅助提取,提取液经GPC柱净化除脂,GPC浓缩液用氮气吹至尽干,然后用乙酸酐和吡啶衍生化,最后,衍生化物经GC色谱柱(HP-5MS,30 m×0.25mm,0.25μm)分离,在SIM模式下进行定性和定量分析。6种类固醇激素以外标法定量,在10~500μg/kg线性范围内相关系数(r)均大于0.999;方法的定量限LOQs(S/N≥10)为4~10μg/kg;添加水平为10μg/kg、50μg/kg、200μg/kg时,加标回收率范围为77.2~112%,相对标准偏差为4.2~10%。结果表明,所建方法准确、可靠,已成功用于黄油中6种类固醇激素的检测分析。     

Multi-residue method for the confirmation of four avermectin residues in food products of animal origin by ultra-performance liquid chromatography-tandem mass spectrometry

A confirmatory method was developed for the rapid determination of abamectin, ivermectin, doramectin and eprinomectin residues in various food products of animal origin, such as pork muscle, pork liver, fish and milk. Samples were homogenized, extracted and de-proteinized by acetonitrile, cleaned via two-step cleaning procedure using Bond Elut C(18) SPE columns and then alumina-N cartridges. All the four avermectin residues in different animal-food products were simultaneously separated and determined by ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) within 3.5 min. Data acquisition under positive ESI-MS/MS was performed by applying multiple reaction monitoring (MRM) for both identification and quantification, and mass spectrometric conditions were optimized to increase selectivity and sensitivity. The matrix-matched calibration curves for different matrices, such as pork muscle, pork liver, fish and milk, were constructed and the interference effect of different sample matrices on the ionization was effectively eliminated. The UPLC-MS/MS method was validated with satisfactory linearity, recovery, precision and stability. Matrix-matched calibration curves of abamectin, ivermectin, doramectin and eprinomectin in four different matrices were linear (r(2)( )≥ 0.990, goodness-of-fit coefficients ≤12.8%) in the range 2.5-200 μg kg(-1). The limits of detection and quantification for the four avermectins were in the range 0.05-0.68 and 0.17-2.27 μg kg(-1), respectively. Recoveries were 62.4-104.5% with good intra- and inter-day precision. The method was rapid, sensitive and reliable, and can be applied to the quantitative analysis of avermectin residues in different animal-food products.     

Tumours induced in Fischer 344 rats by the feeding of disulfiram together with sodium nitrite

A mixture of 0·1% disulfiram together with 0·2% sodium nitrite in powdered rat diet was fed to 20 male and 20 female Fischer 344 rats for 78 wk, after which the animals were observed until death. Ten of the males and 12 of the females died with tumours of the oesophagus, tongue, squamous stomach and nasal cavity. None of these tumours was observed in rats fed either disulfiram or sodium nitrite alone at similar doses. The tumours were attributed to the reaction of disulfiram and nitrite in the stomach, with the formation of nitrosodiethylamine, which has given rise to these tumours in Fischer rats from the same colony.     

生物传感器在生物毒素检测中的应用进展

生物传感器技术是一种全新的微量分析技术, 通过生物传感器进行检测可以实现高通量、高精确度、快速筛查及定量分析等目标, 本文介绍了生物传感器的原理、分类及其在真菌毒素、细菌毒素检测中的应用现状, 并讨论了所存在的问题和未来的发展展望。