微波消解-电感耦合等离子体质谱测定食品中硒的含量

建立微波消解-电感耦合等离子体质谱(ICP-MS)测定食品中硒元素的方法,样品经微渡消解后,采用Re元素为内标,用电感耦合等离子质谱测定样品硒元素的含量.用该方法对国家标准物质灌木枝叶(GBW603)和对虾(GBW08572)及国际标准物质角鲨肉(DORM-2)和龙虾肝胰脏(TORT-2)进行分析,所得结果与其参考值吻合较好,硒元素的检出限为0.18μg/L,3次测定的RSD<5%.将海带、豆芽、大蒜、洋葱在硒的溶液中培养一段时间,测定培养前后硒的变化,发现这些植物对硒均有富集作用.对市场上的一些富硒产品进行硒含量的检测,发现鸡蛋清中的硒含量为10.4mg/kg,高于鸡蛋黄中硒的含量7.4mg/kg.     

深圳居民膳食中硒的测定及其摄入量评估

检测了深圳市居民膳食中硒的含量,并进行统计分析。结果表明,深圳市居民膳食中常见食品的硒含量范围在0~196 mg/100 g,其中,硒含量高低水平为:水产品肉类蛋及其制品鲜(干)食用菌坚果籽类豆类及其制品鲜(干)藻类谷物乳制品谷物制品蔬菜。深圳市外来劳务工的日均硒摄入量为77.9 mg/d。其中,硒摄入量的主要来源为肉类,硒摄入贡献率分别为46.5%,种类较单一。深圳市常住居民的日均硒摄入量为128.9 mg/d,高于外来劳务工的硒摄入水平,且主要来源丰富,分别是肉类和水产类,硒摄入贡献率分别是42.9%和25.8%。研究结果为深圳市加强劳务工营养膳食指引和科学补硒提供参考。     

异丙醇基体改进剂用于微波消解-ICP-MS测定芹菜、圆白菜、鸡肉和猪肝中微量硒

目的:采用异丙醇作为基体改进剂,建立微波消解-ICP-MS测定芹菜、圆白菜、鸡肉和猪肝中微量硒的方法。方法:样品经以6 m L硝酸+2 m L过氧化氢作为消解试剂进行微波消解,以2%异丙醇作为基体改进剂,锗元素进行内标校正,用ICP-MS的碰撞池技术测定硒元素含量。结果:该方法拟合系数为1.0000,检出限为0.3μg/kg,定量限为1μg/kg。通过有证标准物质对方法进行验证,结果均在证书值范围内。该方法线性好、检出限低、准确可靠,可用于食品中硒元素的准确测定。     

湿法消解-电感耦合等离子体发射光谱法检测富硒豆类中硒蛋白含量

目的 结合不同提取方式建立湿法消解-电感耦合等离子体发射光谱法(inductively coupled plasma optical emission spectrometry, ICP-OES)检测富硒豆类中硒蛋白含量的方法。方法 分别以水、0.5 mol/L氯化钠溶液、75%乙醇(V:V)、0.1 mol/L氢氧化钠溶液为溶剂, 超声辅助提取富硒豆类中的硒蛋白, 硝酸-过氧化氢体系湿法消解样品, 采用ICP-OES检测硒蛋白含量。结果 以氢氧化钠溶液作提取剂, 硒元素分析谱线为196.0 nm, 检测效果最佳, 线性关系良好, 相关系数大于0.99, 检出限为0.082 mg/kg, 定量限为0.272 mg/kg。硒标准溶液的加标回收率为90.0%~98.5%, 相对标准偏差为3.1%~6.3%, 硒代蛋氨酸标准溶液的加标回收率为84.0%~92.8%, 相对标准偏差为0.2%~1.8%。结论 该方法前处理提取效果好, 湿式消解法消解样品完全,方法的物理化学干扰少, 具有良好的准确度和精密度, 适用于富硒豆类食品中硒蛋白含量的准确检测。     

常见干豆类及豆制品中嘌呤含量研究

目的:检测常见干豆类及豆制品中的嘌呤含量,为高尿酸血症与痛风患者健康膳食提供指导。方法:采用高效液相色谱法测定嘌呤含量,色谱柱选用Waters Atlantis T3柱(4.6mm×250mm×5μm),流动相为10.0mmol/L甲酸铵(pH3.6)和甲醇(99%∶1%),流速1.0mL/min,柱温30℃,检测波长254nm。结果:不同种类干豆及豆制品中嘌呤含量具有显著差异,干豆类中嘌呤含量显著高于豆制品;干豆类中,蚕豆最高。豆制品中,豆粉最高。结论:不同种类干豆及豆制品中嘌呤含量有差别;干豆类普遍高于豆类制品。     

固相萃取-气相色谱串联质谱法测定肉及肉制品中11种农药残留

依据全国食品中农药残留近年的检测状况,建立了一种快速有效的肉及肉制品中11种常用农药的残留检测方法。肉及肉制品样品中残留农药用乙腈提取,经冷冻离心和PSA/Silica固相萃取柱净化后,采用气相色谱-质谱联用仪（GC-MS）进行分析检测,内标标准曲线法定量。结果显示,11种农药在0.05～2.00μg/mL浓度区间内线性方程的相关系数均大于0.9950,检出限区间为0.002～0.020 mg/kg,定量限区间为0.005～0.060 mg/kg。在样品中添加0.05、0.10、0.20 mg/kg 3个浓度水平的加标实验中,样品的加标回收率在74.3%～118%之间,相对标准偏差在2.1%～9.6%之间。结果表明,该方法的灵敏度、重复性和稳定性较高,适用于肉及肉制品中11种农药残留的检测。     

河南省居民肉及肉制品中铜摄入水平及其风险评估

目的以河南省肉及肉制品中铜为例,演示采用简单分布评估方法,评价河南省居民肉及肉制品饮食中铜摄入情况及其潜在的健康风险。方法 2014—2015年在河南省16个省辖市随机采集肉及肉制品309份,按照食品中铜测定的原子吸收光谱法标准操作程序进行检测,结合河南省2010—2012年开展的居民营养与健康状况监测中肉及肉制品的消费量数据,采用简单分布模型(确定性评估)方法,借鉴文献发表的肉及肉制品对膳食中铜的贡献率,计算河南省不同年龄组人群全膳食中铜摄入水平及其潜在的健康风险。结果肉及肉制品中铜的平均含量为0.556 mg/100 g,中位数为0.060 mg/100 g,不同肉及肉制品中铜平均含量最高为内脏(1.561 mg/100 g),铜平均含量最低的为猪肉(0.068 mg/100 g)。河南省居民每天通过进食肉及肉制品的铜平均摄入量为0.046 mg/d,高端(P95)摄入量为0.144 mg/d。利用文献报道的肉及肉制品贡献率外推全膳食中铜摄入量后发现,河南省居民全膳食中铜的平均和P95摄入量分别为0.638和1.977 mg/d。个体评估结果显示,全人群铜摄入量处于推荐摄入量(RNI)与可耐受最高摄入量(UL)之间的个体比例为21.12%(801/3 792),处于EAR和RNI之间的个体比例为8.10%(307/3 792),而低于平均需要量(EAR)、大于UL的人群比例分别为69.75%(2 645/3 792)和1.03%(39/3 792)。结论河南省全人群膳食中铜摄入量缺乏的风险较高,铜过量的风险较低。     

深圳市总膳食中16种邻苯二甲酸酯的污染分布

为深入了解深圳市居民膳食中邻苯二甲酸酯类物质的污染分布规律,利用总膳食研究方法对深圳市膳食样品进行处理,采用气相色谱-质谱法分析膳食混样及单样中的16种邻苯二甲酸酯类含量,评估其污染状况。结果显示,混合膳食样品中深圳市城区的DMP、DBP、DIBP、DEP及DEHP的最高含量分别为0.0672,0.3304,0.3590,0.4537,0.4588 mg/kg;农村区DMP、DBP、DIBP、DEP及DEHP的最高含量分别为0.4347,1.8357,0.5051,0.0909,6.1565 mg/kg。城区DEP、DEHP的污染较DMP、DIBP及DBP污染严重,农村区DBP、DEHP的污染较严重。薯类及制品、肉类及制品、蛋类及制品和水产类及制品4类食品的PAEs的污染程度相对较高。单个样品中,黄鳝中DEP的污染程度最高,为14.5378 mg/kg;马铃薯片中DMP的含量最高,为0.8525 mg/kg;鲫鱼中DEHP的含量最高,为13.3437 mg/kg;鹌鹑蛋中DIBP和DBP污染程度较高,分别为0.8562,2.3118mg/kg。相比于国内外报道的数据,深圳市膳食中PAEs整体污染处于较低水平。     

不同发酵豆制品中生物胺调查分析

目的 调查腐乳、豆酱和豆豉3类豆制品中生物胺含量, 初步了解发酵豆制品中生物胺存在情况。方法 参照GB 5009.208-2016《食品安全国家标准 食品中生物胺的测定》, 采用高效液相色谱法测定6种腐乳、3种豆酱、6种豆豉中的生物胺含量。结果 腐乳中的生物胺含量明显超出另两类, 其总生物胺平均含量达472.35 mg/kg; 豆酱略高于豆豉, 分别为196.77 mg/kg和171.46 mg/kg。腐乳、豆豉和豆酱样品中含量最高的生物胺均是酪胺, 腐乳样品中居其次的是腐胺, 豆豉和豆酱样品中是章鱼胺, 3种品种样品亚精胺和精胺含量均较少。结论 从整体而言, 3类发酵豆制品生物胺含量在安全范围内。     

豆类、坚果及籽类中硼本底含量调查研究

食品中硼元素本底值对于判断食品中是否添加硼砂或硼酸至关重要。本文使用电感耦合等离子体质谱法(ICP-MS)对硼本底值含量较高的豆类、坚果及其籽类进行测定,旨在为食品安全监管判定非法添加行为提供数据支持。检测结果显示,豆类、坚果及籽类中硼的本底含量相比于文献报道的蔬菜、水果、肉类等食品均较高。     

Nickel content of various Dutch foodstuffs

The nickel content of 260 samples from various types of foods available in the Netherlands was measured by means of flameless atomic absorption spectrometry. In most samples the nickel content was found to be less than 0.5 mg/kg. Two products contained considerably more nickel than all the other foodstuffs, viz. nuts and cacao products, in which nickel concentrations up to 5.1 and 9.8 mg/kg, respectively, were measured. Occasionally nickel contents above 1 mg/kg were found in margarine and sauces.     

电感耦合等离子体质谱法测定乳制品中硒含量

本研究建立以甲醇为基体改进剂内标校正外标定量的电感耦合等离子体质谱法检测乳与乳制品中微量元素硒的含量。本研究采用微波消解前处理方法,使用电感耦合等离子体质谱仪的碰撞反应模式,内标中添加甲醇溶液为基体改进剂,通过分析微量元素硒的6个同位素的灵敏度和线性相关性,确定选择质量数 _⁷⁸Se 测定乳制品中的硒。同时用Minitab 中的DOE实验设计进行分析,采用 _⁷²Ge元素作内标补偿基体效应,最终以 7.5 %(V/V)的甲醇作为基体改进剂,有效的控制了硒的回收率；本研究的方法检出限为固体样品0.00737mg/kg,液体样品0.00264mg/kg,5种不同基质样品的精密度(RSD,n=6)在2.0 %～6.1 %之间,加标回收率为 81.1 %～117 %。该检测方法快速简便,精密度高,准确性好,也具有较高的灵敏度,可为乳及乳制品中微量元素硒的测定提供参考。     

昆明市售坚果中5种有害元素的监测

目的了解昆明市售坚果中铅、砷、汞、铬、镉5种有害元素的污染情况。方法昆明市14个区县采集共140份坚果,采用浓硝酸为消解液,石墨消解仪对样品进行前处理消解,电感耦合等离子体质谱同时测定坚果中的5种有害元素的含量,内标法定量。结果样品中汞、镉、砷、铅及铬的检出率依次为35%、45%、65%、100%和100%。从坚果类别分析,检出率为葵花籽(81.2%)花生(80%)松子(77.5%)南瓜子(67.5%)西瓜子(61.3%)开心果(60%)=葡萄干(60%)杏仁(58.7%)核桃(48.3%),从有害元素含量分析,检测含量为铬(0.961 mg/kg)砷(0.057 mg/kg)铅(0.053 mg/kg)镉(0.047 mg/kg)汞(0.009 mg/kg)。2份样品中铅元素含量超过标准限值,超标率为1.4%。结论样品有害元素的含量较低,但检出率较高,相关部门应加强对坚果在贮存、加工、包装过程中的监督管理,保障消费者的食品安全和健康。     

Predicted dietary intake of selenium by the general adult population in Belgium

The total selenium content of about 800 food products purchased in Belgium was determined and combined with food records to determine the nutritional selenium status of Belgian people. The largest selenium concentrations (>1?mg?kg^?1) were found in Brazil nuts and offal, of which the consumption is limited. Usually consumed food groups with the highest selenium concentrations were fish and shellfish (0.2–0.9?mg?kg^?1), eggs, poultry meat, cheese, mushrooms and pasta (approximately 0.2?mg?kg^?1). The mean dietary selenium intake was calculated to be 60?µg?day^?1, which is at the lower end but within the range recommended by the Superior Health Council in Belgium (60–70?µg?day^?1), and adequate according to the 55?µg?day^?1 recommended by the Scientific Committee on Food (SCF) of the European Commission. The major sources of selenium intake are meat and meat products (31%), fish and shellfish (20%), pasta and rice (12%), and bread and breakfast cereals (11%).     

Ochratoxin A in conventional and organic cereal derivatives: a survey of the Italian market, 2001-02.

Ochratoxin A is a mycotoxin produced mainly by Penicillium verrucosum and Aspergillus ochraceus. Although typically considered a cereal contaminant, it has also been detected in dried fruit, nuts, meat and derivatives. To estimate the quantity of ochratoxin A that might be ingested by Italian consumers from these foods, 211 cereal derivatives (flours and bakery products) were analysed by high-performance liquid chromatography. Products were from conventional and organic agriculture and from integrated pest management agriculture. All commercial flours and derivatives examined contained ochratoxin A at concentrations very much below the legal limit (3 microg kg(-1)): the highest value, 0.816 microg kg(-1), was detected in a sample of spelt whole flour from organic agriculture. In many samples, the ochratoxin content was below the limit of detection; only rarely did values exceed 0.5 microg kg(-1). In baby foods, four samples were above the particularly restrictive Italian legal limit of 0.5 microg kg(-1). Although some significant differences were found between samples from conventional and organic agriculture when some product categories were examined (namely, baby foods as semolina and rice creams), no important difference was found between the two types of agricultural practice when all types of cereal derivatives were considered together.     

Cadmium in blue poppy seeds and poppy seed-containing products

Blue poppy seeds, semi finished products and finished baked goods with poppy seeds, were analyzed for cadmium by atomic-absorption spectrometry. The average content was 0.739 mg/kg (median 0.654 mg/kg) for poppy seeds, 0.317 mg/kg (median 0.366 mg/kg) for semi finished products and 0.107 mg/kg (median 0.088 mg/kg) for baked goods. Poppy seeds therefore must be considered as one of the most cadmium contaminated foods. For consumers, especially children, recommendations for consumption should be established.     

Validation of UPLC method on the determination of formaldehyde in smoked meat products

The study was carried out to establish a formaldehyde (FA) detection method in smoked meat products with ultra-performance liquid chromatography (UPLC) method. The high-performance liquid chromatography method was developed by using steam distillation as extraction method and then derived by2,4-dinitrophenylhydrazine (DNPH). The final optimum conditions of derivatization for UPLC method were determined as follows: DNPH dosage of 0.3 mL, derivatization temperature of 60°C, derivatization time of 60 min, and twice extraction. This method was further applied to determine the content of FA in the smoked meat products from five companies. The internal FA in the smoked meat products ranged from 25.55 mg/kg meat to 49.20 mg/kg meat, and the surface FA was 34.04 mg/kg meat to 165.25 mg/kg meat. Thus, this study establishes a simple, fast, and reliable method for the analysis of FA in smoked meat products.     

Copper content of commonly consumed food in Brazil

Little is known of copper content of Brazilian food. In this paper, copper contents of several typical Brazilian foods were determined. The samples were bought in retail stores in cities of the southeast region of Brazil. Atomic absorption spectrophotometry with wet oxidation of the organic material was employed. The highest copper content was found in beef liver (6.06 mg/100 g of fresh product). Lowest copper content was found in milk and in fish fillet, with values below 0.01 mg/100 g of fresh product. Crude beans, Nescau^TM and whole wheat had copper contents from 0.44 to 1.04 mg/100 g of fresh food. Other foods, such as fruits, vegetables, grain products, baked products, roots and meat products had copper contents varying from 0.02 to 0.41 mg/100 g.     

硒强化剂的急性和蓄积毒性试验研究

为安全生产补硒保健食品和保障食品安全提供科学参考依据.用保健食品常见的硒强化剂亚硒酸钠对小鼠进行不同剂量灌胃,通过急性和蓄积性毒性试验, 系统研究硒对小鼠生长性能,组织病理变化,血常规、血液生化指标等的影响,建立小鼠硒中毒的动物模型.急性毒性试验表明:小鼠经口LD50为3.86 mg/kg;蓄积性毒性试验表明亚硒酸钠对小鼠有弱蓄积性.     

Selenium content in selected Slovenian foodstuffs and estimated daily intakes of selenium

Food is the primary source of selenium for man and, since selenium is an essential trace element, the nutritional selenium status is of importance. Data on this topic are currently lacking in Slovenia. In the present study, selenium contents of some selected foods purchased on the Slovenian market were determined and estimation of the daily dietary intake by analysing 20 diet samples collected in four Slovenian Army barracks was made. In determination of the selenium content in selected food, the highest values were found, as expected, in protein-rich food such as fish, meat and eggs (33–686 ng g⁻¹), but lower values in milk and dairy products (12–30 ng g⁻¹) and vegetables and fruits (0.3–77 ng g⁻¹). Analysis of 20 military total daily diet samples, gave an average selenium daily intake of 87 μg.