玉米中黄曲霉毒素B1测定的不确定度评定

采用超高效液相色谱法对玉米中黄曲霉毒素B1的不确定度进行评估。根据CNAS-GL006-2018《化学分析中不确定度的评估指南》和JJF1059.1-2012《测量不确定度评定与表示》中的有关规定,建立测定玉米中黄曲霉毒素B1不确定度的数学模型,逐层对不确定度来源进行分析。通过对不确定度分量进行量化和合成,得出当玉米中黄曲霉毒素B1为3.60μg/kg时,其相对扩展不确定度为0.14μg/kg(k=2)。结果表明,影响检测结果的主要因素为样品非均匀性、回收率、校准过程及样品处理液定容;其量化结果分别为0.0140、0.009、0.007、0.0058。     

2种高效液相色谱仪测定芝麻酱中黄曲霉毒素B1的不确定度评定

目的评定并比较2种厂家高效液相色谱仪测定芝麻酱中黄曲霉毒素B_1的不确定度。方法分别采用Agilent1260型及Thermo U3000型高效液相色谱仪测定芝麻酱中黄曲霉毒素B1的含量,应用不确定度理论分析检测数学模型,对测定不确定度的来源进行分析和量化。结果结果表明当黄曲霉毒素B_1的测定结果(Agilent 1260、Thermo U3000)分别为6.1236、6.0230μg/kg时,其扩展不确定度分别为0.42706、0.31115μg/kg,k=2。结论标准溶液的配制、由最小二乘法拟合标准曲线计算样品浓度以及回收率测定引入的不确定度对结果影响较大。在本实验条件下, Agilent1260型测定引入的相对不确定度大于Thermo U3000型测定引入的不确定度,后者仪器更加稳定,结果更准确。     

粮油中黄曲霉毒素B1的监测

利用简单的仪器设备监测粮油中的黄曲霉毒素B1，此法直接、快速，利于推广普及。     

二氧化氯对霉变玉米黄曲霉毒素B1脱毒效果的研究

霉变染有黄曲霉毒B1（AFB1）的玉米,用低浓度（250μg/ml）二氧化氯浸泡30－60min,能有效地解除AFB1的毒性。比较了二氧化氯作用时间及不同产地产品脱毒效果的差异,对二氧化氯的解毒功效及其使用安全性也作了探讨。     

米扁虫对玉米中黄曲霉毒素B1含量影响的研究

了解在非霉变和不产毒的储存条件下,原粮中昆虫对真菌毒素含量的影响具有重要生态学意义。测定了含黄曲霉毒素B1(AFB1)的玉米分别接入15、45和135头/kg米扁虫幼虫和成虫后不同存放时间AFB1含量。结果表明,米扁虫幼虫和成虫接入一定时间后均可导致玉米中AFB1含量和霉菌总数显著降低,米扁虫成虫对AFB1含量降低的作用大于幼虫,玉米破碎粒率越低时AFB1含量降低越显著,虫口密度越大、接入时间越长,AFB1含量降低越显著。     

臭氧降解玉米中黄曲霉毒素B1效果及降解动力学研究

玉米是我国重要的食品和饲料原料,当收获、加工和储藏等措施不当时,可能会造成黄曲霉毒素B1（aflatoxin B1,AFB1）污染玉米这一突出问题,AFB1已被国际癌症机构定为1级致癌物。尽管目前已建立了一些物理、化学和生物降解AFB1的方法,但高效、安全、经济的绿色降解方法仍很少。本研究以AFB1污染的玉米为试样,研究臭氧对玉米中AFB1的降解效果。结果表明：AFB1降解率随着臭氧质量浓度的增加和处理时间的延长而显著提高;当水分质量分数为20.37%的玉米经90 mg/L的臭氧处理40 min后,AFB1含量由77.6 μg/kg降低到21.42 μg/kg,降解率达72.4%。臭氧降解AFB1的动力学模拟结果表明,臭氧降解AFB1符合一级动力学模型。玉米中AFB1降解速率常数按以下次序递减：k90 mg/L＞k65 mg/L＞k40 mg/L。实验得到臭氧降解AFB1的动力学方程、反应速率常数、决定系数和半衰期,为最优地控制臭氧降解AFB1的反应条件奠定了理论和实践基础,也为臭氧降解AFB1污染玉米的应用提供了技术保障。     

食品中黄曲霉毒素B1污染研究进展

农作物（包括玉米、小麦等）在生长、收获和储存的过程中,容易受到产毒真菌及其代谢毒物（霉菌毒 素）的污染;其加工形成的粮、油等食品及被污染饲料饲养所得的畜产品进入食物链后,易引发人类急、慢性中 毒。黄曲霉毒素B1是众多霉菌毒素中较常见且毒性较高的一种,过量摄入具有致癌、致畸形、免疫抑制等毒性效 应。本文综合国内外研究进展,从食品中黄曲霉毒素B1污染发生的来源及影响因素、黄曲霉毒素B1的分子结构与毒 性、致病机理、限量标准、风险评估及防控等方面对食品中黄曲霉毒素B1污染展开综述。     

黄粒米中黄曲霉毒素B1的调查

黄粒米中黄曲霉毒素Ｂ_１的调查吉林粮食高等专科学校王晓英前言１９９５年夏，长春市售部分大米黄粒米含量高达１０％左右，超过国家标准。随着有关黄曲霉毒素知识的普及，部分人误认为黄粒米是黄曲霉污染所造成，黄粒米含有黄曲霉毒素，甚至误认为黄粒米会致癌。为了澄?..     

分级制备法评估粉碎粒径对玉米中黄曲霉毒素B1测定的影响

评估粉碎粒径对黄曲霉毒素B1（AFB1）测定的影响,改进样品制备方法,提高现行国标检测方法对玉米原粮样品AFB1测定结果的重复性。以天然AFB1阳性玉米为实验材料,采用分级制备方式得到不同粒径范围的四个级别样品,使各级样品的粒径分布差异最大化,通过各级别样品中AFB1测定值及变异系数评估样品制备对AFB1测定值的影响,得到最佳样品制备要求和称样量,进行验证。样品粉碎后的不同粒径样品与该部分的AFB1含量成反比;当称样量为5 g时,应将样品粉碎至全部通过0.6 mm网筛;当称样量为10 g时,应将样品粉碎至全部通过0.9 mm网筛,以使检测结果重复性符合GB/T 32465—2015《化学分析方法验证确认和内部质量控制要求》的要求。研究结果兼顾AFB1测定准确性与操作效率,可扩大应用于其他真菌毒素的检测,对完善食品中真菌毒素检测方法具有参考意义。     

黄曲霉毒素B1检测方法的分析

黄曲霉毒素B1是一种致癌物质 ,许多国家已将其限量标准提高 ,黄曲霉毒素B1检测方法的检出限已因其毒性而提高 ,并已成为国际贸易中新的技术壁垒。文中介绍了黄曲霉毒素B1的几种常见检测方法 ,并对其特点及检出限进行了概括性的分析。     

芝麻素标准样品的研制

依据GB/T 15000.3—2008《标准样品工作导则》,研制芝麻素标准样品。以芝麻为原料,采用高速逆流色谱法分离制备芝麻素单体,通过UV、IR、MS和NMR等手段进行结构表征,同时进行薄层色谱鉴别和热重分析。芝麻素样品进行了均匀性检验、稳定性检验和8家实验室联合定值。结果表明:该样品均匀性良好,在0~4℃条件下储存36个月稳定性良好,定值结果确定其标准值为99.73%,置信度95%的不确定度为0.20。成功研制出了芝麻素国家标准样品,达到了GB/T 15000.3—2008规定的技术要求,样品具有溯源性,可用于芝麻素及相关产品的质量控制和检测方法评定。     

小麦粉标准物质的研制

目的研制均匀性和稳定性符合要求的4种小麦粉标准物质,用于小麦的质量控制。方法将制备的成品经灭菌处理后于温度小于26℃、湿度小于60%的避光房间保存。采用电感耦合等离子体光谱法和质谱法对标准物质候选物的均匀性和稳定性进行考察。同时选取9家具有丰富定值经验的实验室对其化学成分进行协作定值。结果确定了4种小麦粉标准物质中Cr、As、Cd、Hg、Pb、Ni、Cu、Se、K、Na、Ca、Mg、Mn、Fe、Zn和Al共16个元素的标准值和不确定度。结论结果表明此4种标准物质的均匀性、稳定性、标准值的不确定度评定过程都达到JJF 1006-94《一级标准物质》相关技术要求,已被批准发布为国家级标准物质。     

In vivo toxicity assessment of aflatoxin B1-contaminated corn after ozone degradation

Corn is an important food and feedstuff in China and worldwide. The problems caused by aflatoxin B₁-contaminated corn (ACC) are of great concern. Our previous studies have demonstrated that ozone can effectively degrade AFB₁ in corn, prompting us to investigate the in vivo toxicity of treated ACC. In this study, 35 Kunming mice were used to assess the in vivo toxicity of ozone treated ACC. Results indicated that compared to mice fed with basal feedstuff (provided by the Shanghai SLAC Laboratory), those fed with ACC have significantly decreased mean weight as well as total protein (TP), albumin (ALB), and globulin (GLB) contents (p < 0.05). On the other hand, the liver and kidney/body weight ratio as well as the serum alanine transaminase (ALT), aspartate aminotransferase (AST), and alkaline phosphatase (ALP) levels significantly increased (p < 0.05). Obvious histopathological changes were found in the liver and kidney. When mice were fed with the ozone-treated ACC, no significant differences were observed in the mean weight, the liver and kidney/body weight ratio and in the major serum indexes ALT, TP, ALB, and GLB (p > 0.05). However, AST and ALP significantly increased (p < 0.05), and slight histopathological changes were found in liver tissues. This study indicated that ACC may lead to significant changes in various physiological characteristics and biochemical indexes in liver and kidney tissues, but ozone treatment of ACC could significantly reduce these changes.     

Aflatoxin M1 in milk powders: Processing, homogeneity and stability testing of certified reference materials

As part of the certification campaign of three candidate reference materials for the determination of aflatoxin M₁ (AfM₁) in whole milk powders, homogeneity, short- and long-term stability tests of naturally contaminated milk powders have been performed. The homogeneity of two AfM₁-contaminated milk powders was studied by taking samples at regular intervals of the filling sequences and analysing in triplicate for their AfM₁ contents by liquid chromatography with fluorescence detection (LC-FLD) using random stratified sampling schemes. The homogeneity testing of an AfM₁ 'blank' milk powder material was performed by determining the nitrogen content because AfM₁ levels were below the limit of detection of the most sensitive determination method. The short-term stability of AfM₁-contaminated milk powders was evaluated at three different storage temperatures (4, 18 and 40°C). After storage times of 0, 1, 2 and 4 weeks, samples were investigated using LC-FLD. The long-term stability study comprised of measurements after 0, 6, 12 and 18 months after storage at -20 and 4°C. Analyses were done by LC-FLD. Based on the homogeneity tests, the materials were sufficiently homogenous to serve as certified reference materials. Corresponding uncertainty contributions of 0.23-0.89% were calculated for the homogeneity. The stability measurements showed no significant trends for both short- and long-term stability studies. The long-term stability uncertainties of the AfM₁-contaminated milk powders were 7.4 and 6.3%, respectively, for a shelf-life of 6 years and storage at -20°C. Supplementary stability monitoring schemes over a long period of several years are currently ongoing.     

Degradation of aflatoxin B1 in peanut meal by electron beam irradiation

The effects and safety of electron beam irradiation (EBI) treatment on the detoxification of aflatoxin B₁ (AFB₁) in the peanut meal were evaluated in this article. The AFB₁ degradation was predominantly affected by both initial AFB₁ and water concentrations. The degradation of AFB₁ in the selected concentrations (0.5–5 ppm) was proven to follow pseudo first-order reaction kinetics (R² > 0.95). The AFB₁ degradation was faster when the initial concentration was 5 ppm and the moisture content was 21.47%, in comparison with the initial concentration of 1 ppm and 0.5 ppm and the moisture content of 14.32% and 8.74%, respectively. The Ames and cytotoxicity tests were employed to evaluate the residual toxicity of EBI-treated peanut meal. The mutagenic activity of EB-treated samples was completely lost compared with that of untreated samples and the degradation products in peanut meal has almost no cell toxicity.     

时间分辨荧光免疫法检测食品中黄曲霉毒素B1的含量

目的建立高灵敏度的时间分辨免疫法检测黄曲霉毒素B_1的含量。方法通过双功能螯合剂异氰酸苄基二乙烯三胺四乙酸络合稀土元素Eu~(3+)标记抗AFB_1的单克隆抗体,以AFB_1-OVA为固相抗原,优化反应条件,建立直接竞争时间分辨免疫检测方法。结果优化条件后,方法灵敏度为0.02μg/L,IC_(50)为0.73μg/L,线性检测范围为0.01~30μg/L,大米、花生、黄豆和干果样品回收率在91%~104%之间,检测结果准确;与结构类似物AFB_2、AFG_1、AFG_2、AFM_1的交叉反应率分别为17.3%、4.49%、2.37%和0.73%。结论本方法灵敏度高、特异性强、检测快速,可以满足实际样品的检测需求。     

酶联免疫吸附法测定云南铁皮石斛中黄曲霉毒素B1

目的建立酶联免疫吸附法测定铁皮石斛中黄曲霉毒素B_1(afatoxin B_1, AFB_1)的分析方法,并研究酶联免疫吸附法(enzyme-linkedimmunosorbentassay,ELISA)和高效液相色谱法(highperformanceliquid chromatography, HPLC)测定云南铁皮石斛中AFB_1的结果差异性。方法用甲醇+水溶液(50+50, V/V)提取石斛中AFB_1,采用酶联免疫吸附法和高效液相色谱法同时检测云南铁皮石斛(铁皮枫斗)中AFB_1,进行准确性、精密度和回收率等方法学实验,比较2种方法的差异性。结果 ELISA法在测定范围内AFB_1与其对应的吸光度值之间呈良好的线性关系,回归方程Y=-34.798X+18.134,相关系数r~2为0.9967;添加1.0、4.0、10.0μg/kg3个浓度的平均加标回收率为85.3%～94.7%,相对标准偏差为2.57%～4.88%。2种方法的结果符合率为93.2%～117%,相对标准偏差均小于10%。结论 ELISA法具有操作简单、检测速度快、灵敏、特异性好等优点,可同时检测大批量样品中AFB_1的含量。     

酶联免疫法检测复合调味料中黄曲霉毒素B1含量

目的酶联免疫法(enzyme-linked immunosorbentassay,ELISA)快速检测复合调味料中黄曲霉毒素B_1的含量。方法用70%甲醇水溶液提取非含油型复合调味料中的黄曲霉毒素B_1待测液,含油型复合调味料则首先加入石油醚将油萃取出来,后加入70%甲醇水溶液抽提。使用酶联免疫法进行定量限、回收率与重复性等实验。结果使用不同前处理的检测结果的定量限为3μg/kg,相对标准偏差分别为2.06%和2.73%;回收率范围在90%～110%之间;重复性平均值分别为10.77μg/kg和10.84μg/kg,相对标准偏差分别为3.89%和2.44%。结论复合调味料通过不同的前处理方法,后使用酶联免疫法检测复合调味料中黄曲霉毒素B_1结果准确,重复性较好。     

一种含毒死蜱的黄瓜冻干粉基质标准物质的研制

目的建立了一种以黄瓜为基质的毒死蜱标准物质的制作方法。方法黄瓜样品经研磨、加标、冷冻干燥、磨粉、混匀、真空包装后,用GB 23200.113-2018检验样品的均匀性、稳定性,并联合多家实验室对黄瓜冻干粉中毒死蜱基质样品定值,同时分析样品的不确定度。结果F-检验法和t-检验法表明在95%置信区间内,样品均匀性、短期稳定性和长期稳定性均达到标准物质要求。采用格拉布斯和柯克伦检验对定值结果进行异常值检验,并对结果进行不确定度评估,样品定值为1.78 mg/kg,不确定度为0.12 mg/kg。结论该样品具有良好的均匀性、稳定性,可作为蔬菜中毒死蜱含量检测使用的标准物质。     

食品检测用单核细胞增生李斯特氏菌标准物质的研制

目的建立食品检测用单核细胞增生李斯特氏菌标准物质的制备方法,研制均匀稳定的标准物质。方法利用冷冻干燥法制备103 CFU/样品的标准物质,参照CNAS-GL 29《标准物质/标准样品定值的一般原则和统计方法》,抽取20件样品,利用平板计数法测定标准物质的均匀性,并对结果进行统计分析;将样品分别置于-20、25、37℃条件下保藏,对其储藏稳定性和运输稳定性进行评价。组织5家实验室进行协同标定,使用30种即食熟肉制品作为基质,并按照国标法检验标物物质的适用性。结果采用单因素方差分析进行均匀性检验, F=0.922,符合标准物质的要求。标准物质在-20℃保藏28 d, 25、37℃保藏7 d,样品仍然稳定。经5家实验室协同标定,样品含量均在103 CFU/样品的水平;标准物质加入到30种即食熟肉制品中,均可以检出单核细胞增生李斯特氏菌。结论本研究所制备的单核细胞增生李斯特氏菌标准物质的均匀性、储藏稳定性和运输稳定性均符合要求,适用性良好,可用于食品检测实验室的质量控制和食品中单核细胞增生李斯特氏菌检测结果的评价。