紫外吸光光度法测定蔬菜鲜样中硝酸盐氮

采用紫外吸光光度法测定蔬菜鲜样中硝酸盐含量，该法适用于不同硝酸盐含量的蔬菜样品测定，与传统的酚二磺酸法相比，该法精密度和准确度高、操作简便，具有较大的推广价值。     

光化学动力学法测定硝酸盐和亚硝酸盐

本文研究了甲基橙动力学法测定水、食品及蔬菜中硝酸盐和亚硝酸盐。在紫外光照射下甲基橙退色程度与硝酸盐和亚硝酸盐含量成正比。文中提出首先测定二者的总量,然后在氨基磺酸存在下测定硝酸盐的量,再差减求得亚硝酸盐的量。     

蔬菜中硝酸盐含量快速测定方法研究

研究了蔬菜中硝酸盐含量的简易快速测定法.该法简单快速,不需化学试剂,检测成本低,重现性好,变异系数为4.25%.虽然该速测法较国标法测定的结果偏高,考虑到国标法操作较复杂费时,速测法的结果可通过校正系数加以修正,因此该硝酸盐简易速测法的测定结果仍然具有一定的指导意义,特别适用于蔬菜生产和销售企业对蔬菜中硝酸盐含量进行现场日常监控.     

离子色谱法测定蔬菜中硝酸盐含量

１引言 蔬菜易于富集硝酸盐,人体摄入的硝酸盐的８１．２％来自蔬菜。硝酸盐在动物体内被还原为亚硝酸盐,直接使动物缺氧中毒,引起高铁血红蛋白症,也可间接与次级胺结合形成强致癌物质亚硝胺,从而诱发动物的消化道系统癌变。 有关蔬菜中硝酸盐的测定方法,曾报道过的有水杨酸硝化法,酚二碳酸比色法和紫外光度法等,但用离子色谱法测定蔬菜中的硝酸盐在国内至今未见文献报道。本文采用离子色谱法,对芹莱、白菜、黄瓜３种蔬菜中的硝酸盐含量进行了测定,结果令人满意。２实验部分２．１主要仪器和试剂ＩＬＣ－ｌ型色谱系统（Ｗａｔｅｒ…     

武威市腌菜中亚硝基化合物的测定及其胃癌高发原因的分析

针对武威市胃癌高发的现状，应用高效毛细管电泳法(HPCE)和气相色谱法分别测定了当地居民冬季的蔬菜代用品-腌菜中的硝酸盐、亚硝酸盐以及二甲基亚硝胺、二乙基亚硝按．测定结果如下：当地各种腌菜全部检出硝酸盐、亚硝酸盐．其中40份腌菜中的硝酸盐的最高含量为6．1785g/kg，检出率为100％；亚硝酸盐的最高含量为0．1445g/kg，检出率为65％-75％；20份腌菜中的二甲基亚硝胺(NDMA)的最高含量为47．78μg/kg，检出率为60％-70％；二乙基亚硝胺(NDEA)的最高含量为36．32μg/kg，检出率为45％-65％、而且经常食用腌莱人群的胃液中的硝酸盐和亚硝酸盐含量均明显高于不常食用者、试验数据显示，腌菜中亚硝基化合物含量较高，武威市胃癌高发的原因可能与进食腌菜有关。     

叶菜硝酸盐快速检测方法的研究

依据硝酸盐与二苯胺在浓硫酸介质中反应，生成有色物质的原理，在目视比色法的基础上，建立了一种简便、快捷、可靠的测定叶菜中硝酸盐含量的方法，用于实际样品的测定，结果满意。     

活性炭脱色法测定酱油中硝酸盐

蔬菜中常含有较多的硝酸盐,特别是大量使用含硝酸盐的化肥或土壤中缺钼锰等元素时,可增加植物中硝酸盐的蓄积,并且有许多蔬菜亦能从土壤中浓集更多的硝酸盐。豆类蛋白质含量较高,而蛋白质在微生物作用下也能转变为硝酸盐。当人体摄入过高量的硝酸盐,对健康有害,主要是使儿童血液中变性血红蛋白增加;此外,当人体摄入硝酸盐后,经肠道微生物作用,可转变为亚硝酸盐而出现亚硝酸盐不同程度的毒性作用。酱油是人们生活中比较重要的调味品,其中或多或少含有一定量的硝酸盐,因此测定酱油中硝酸盐很有必要。文献[1]用镉柱法,但费时。本法按文献[2…     

用傅里叶变换近红外光谱和偏最小二乘法测定蔬菜中硝酸盐含量

1　引　　言近红外光谱分析技术 (NIRS)是利用物质在近红外光谱区的光学特性快速测定某种物质中的一种或多种化学成分含量的新技术。它以分析速度快、样品准备简单、从单个光谱可进行多种分析、不破坏样品及没有化学污染等优点 ,已广泛用于众多领域的定量分析及过程控制。被称为是一种绿色、快速、高效、适合在线分析的测试手段。蔬菜是极易富集硝酸盐的作物 ,人体摄入的硝酸盐有 81.2 %来自蔬菜 ,进入人体的硝酸盐可转化为亚硝酸盐 ,使人体缺氧中毒产生高铁血红蛋白症。硝酸盐还是一种潜在的致癌物质 ,因此 ,快速的硝酸盐检测方法对于监…     

粤东7种野菜中硝酸盐、亚硝酸盐及维生素C的测定

测定了粤东产7种野菜中的硝酸盐、亚硝酸盐和维生素C.参考蔬菜中硝酸盐分级评价标准,和我国制定的无公害蔬菜亚硝酸盐限量标准,考虑到各种野菜的维生素C的量,对这7种野菜评价如下：积雪草、天胡荽、南方菟丝子和假的硝酸盐量低于轻度污染水平,亚硝酸盐量低于我国制定的无公害蔬菜亚硝酸盐的限量标准（4.0 mg/kg）,维生素C的含量高或较高,所以,它们属于一级野菜, 可以安全食用;蛇含委陵菜和苍耳由于亚硝酸盐量过高,不宜食用或限量食用;荷莲豆的硝酸盐量高于1440 mg/kg,属于高度污染水平,亚硝酸盐量超过我国制定的无公害蔬菜亚硝酸盐的限量标准,不宜食用或限量食用.     

快速测定水样中的硝酸盐和亚硝酸盐

1 引言 测定硝酸盐的常用比色法有酚二磺酸法和紫外双波长法，但这两者都有一定的缺陷。N-（1-萘基）-乙二胺盐酸盐光度法是一种测定亚硝酸盐的简便、准确的方法，为国内外普遍采用。由于亚硝酸盐和硝酸盐在近紫外区的吸收光谱有重叠而影响硝酸盐在紫外区的测定。去除亚硝酸盐干扰的方法有2种，一种是通过加入氨基磺酸来消除，另一种是先测出亚硝酸盐的浓度，通过校正曲线算出它在紫外区的吸光度，再从总吸光度中扣除，其中后一种方法更合理。但笔者依据后一种思想测定硝酸盐和亚硝酸盐的混合溶液中的硝酸盐含量都较理论值低，而通过多元线性回归方程计算的硝酸盐值比单独用硝酸盐标准曲线计算的结果更好。     

Polarographic determination of nitrate in vegetables

A polarographic method for the determination of nitrate in vegetables is presented. The method is based on the reduction of nitrate to nitric oxide which reacts in solution with colbalt (II) and thiocyanate ions forming an electroactive complex that is reduced at the dropping mercury electrode at -0.5 V (vs. SCE). The nitric oxide is generated outside the polarographic cell by addition of ferrous ammonium sulfate and ammonium molybdate in hydrochloric acid to the previously triturated vegetable matrices. The calibration graph was linear in the range of 2-12x10(-6) mol nitrate. The recovery of nitrate in vegetable matrices (broccoli, kale, lettuce, radish, red beet, spinach, turnip and watercress) varied from 85.4 to 107.4 % and the nitrate content, expressed as sodium nitrate, varied from 751 to 10 806 mg kg(-1) of fresh vegetable. The relative standard deviation for the proposed method is lower than 7% and considering a sample of 5.0 g, the determination limit was 39 mg of nitrate per kg fresh vegetable weight. The precision and accuracy of the polarographic method were comparable to those of the reference spectrophotometric method (official AOAC reference method for the determination of nitrate in foodstuffs).     

分光光度法测定新鲜蔬菜中维生素C的含量

水溶性的维生素C是一种人体必需的营养物质。维生素C是含有烯二醇基的多羟基内酯结构,利用其水溶液在波长265nm处有较强烈的紫外吸收峰,建立了直接用紫外分光光度法测定新鲜蔬菜中维生素C含量的方法。实验结果表明,维生素C的含量在1.0~12.0μg/mL内线性关系良好,线性方程为A=0.066 03c+0.019 74(R2=0.997 51),检出限为0.044μg/mL,样品加标回收率为97.5%~105.4%。方法操作简单,准确度高,对新鲜蔬菜的测定结果令人满意。     

分光光度法测定新鲜蔬菜中维生素C的含量

水溶性的维生素C是一种人体必需的营养物质。维生素C是含有烯二醇基的多羟基内酯结构,利用其水溶液在波长265nm处有较强烈的紫外吸收峰,建立了直接用紫外分光光度法测定新鲜蔬菜中维生素C含量的方法。实验结果表明,维生素C的含量在1.0¹2.0μg/mL内线性关系良好,线性方程为A=0.066 03c+0.019 74(R2=0.997 51),检出限为0.044μg/mL,样品加标回收率为97.5%12.0μg/mL内线性关系良好,线性方程为A=0.066 03c+0.019 74(R2=0.997 51),检出限为0.044μg/mL,样品加标回收率为97.5%¹05.4%。方法操作简单,准确度高,对新鲜蔬菜的测定结果令人满意。     

Determination of nitrite, nitrate, and glucose-6-phosphate in muscle tissues and cured meat by IC/MS

The endogenous nitrate concentration in fresh meat and the residual nitrate and nitrite contents after curing are related to food quality and safety. Most ion chromatography (IC) methods suffer from interferences, especially in fresh meat samples, in which the endogenous nitrate content is low, and in cured meat products, in which other nitrogenous compounds can interfere with the separation of inorganic anions. One of the major classes of interfering compounds in fresh meat are sugar phosphates, which originate from glycolysis during the conversion of muscle glycogen to lactic acid. Nitrate can be separated from interfering compounds with a high-capacity anion-exchange column that was manufactured for use with hydroxide eluents (i.e., hydroxide-selective). This column has a different selectivity than traditional IC columns that use carbonate eluents and facilitates the determination of nitrate in both fresh and cured meats. Nitrate was detected by both suppressed conductivity measurement and mass spectrometry (MS). The identifications of nitrate and glucose-6-phosphate were confirmed by MS detection. The described IC/MS method is robust, sensitive to nitrate concentrations as low as 0.10 mg/kg, and can determine sugar phosphates that are useful for monitoring meat freshness. We successfully used this method to determine nitrate in nearly 100 muscle tissues and cured meat samples.     

A new quantitative and low-cost determination method of nitrate in vegetables, based on deconvolution of UV spectra

A new UV-spectrophotometric method for the determination of nitrate in vegetables is presented. The method is based on the spectral deconvolution: UV spectrum of a sample is considered as a linear combination of absorption spectra, named reference spectra. The combination of a small number of spectra of reference allows to reconstitute the shape of UV spectrum of an unknown sample. There have been several fresh vegetables (lettuce, curly lettuce, oak-leaf lettuce), as well as frozen spinaches that have been tested. The results obtained were comparable to those obtained with the reference HPLC method (official European reference method for the determination of nitrate in foodstuffs). The nitrate content varied from 377 to 3240 mg kg⁻¹ of fresh vegetables, and 545 to 1190 mg kg⁻¹ of frozen spinach. The recovery of added nitrate ranged from 91 to 99%. The results were obtained with a laboratory spectrophotometer and also with a dedicated field-type spectrophotometer. This method does not require almost any consumable, is quantitative and very fast reading with easy and low maintenance.     

Differential pulse polarographic determination of nitrate in environmental materials

Nitrate can be determined with reliable accuracy and sensitivity by differential pulse polarography utilizing the catalytic reaction between nitrate and uranyl ion in the presence of potassium sulphate. The differential pulse polarographic peak-height is proportional to nitrate concentration from 1 to 50 muM. The calculated detection limit for nitrate is 8 x 10(-7)M in pure aqueous solution. The method has been applied to determination of nitrate in fresh snow, and river waters and animal feeds.     

Adsorbing colloid flotation separation and polarographic determination of Mo(VI) in water

A method is described for the flotation and determination of Mo(VI) in water at ng/ml levels. Mo(VI) is preconcentrated and separated by adsorbing colloid flotation employing aluminium(III) hydroxide as collector and sodium lauryl sulphate as surfactant at pH 5.3 ± 0.1. The molybdenum content in the froth is estimated by using the catalytic wave of Mo(VI) in the presence of nitrate by charging current compensated d.c. polarography (CCCDCP) or differential pulse polarography (DPP). The effect of variables such as pH, ionic strength, concentration of collector and surfactant, time of stirring and gas flow-rate on the recovery of Mo by flotation is reported. The effects of various cations and anions on the flotation and determination of Mo are studied. This method is employed for the determination of molybdenum in natural fresh water samples.     

石墨炉原子吸收法直接测定海水中铅的方法探索

目的探索石墨炉原子吸收法直接测定海水中铅的检测方法。方法用硝酸铵稀释海水样品,用硝酸钯和磷酸二氢铵作为基体改进剂,用石墨炉原子吸收法测定了海水中的铅含量。结果通过加标回收的验证,检测结果准确可靠。结论适合用于海水中铅含量的测定。     

离子色谱法测定蔬菜硝酸盐含量

建立了化学抑制电导检测离子色谱法定性定量分析蔬菜硝酸盐含量的方法。阴离子分离柱DionexAS14柱(4mm×250mm),保护柱IonPacAG14(4mm×50mm)。流动相为1.7mmol.L-1NaHCO3,1.8mmol.L-1Na2CO3。流速1.2mL.min-1,自动连续再生抑制装置SRS-ULTRA4mm。线性范围为0.1~100.0mg.L-1,线性关系为0.9997,检出限为0.05mg.L-1。应用此法,测定了多种蔬菜硝酸盐含量。方法操作简单、快速、基体干扰少、灵敏、准确。     

The need for reference materials when monitoring nitrate intake

Whether dietary exposure to nitrate metabolites is detrimental or beneficial to human health has long been a matter of controversy. In spite of no consistent epidemiological evidence, nitrate metabolites are associated with the formation of carcinogenic-nitrosamines and gastric cancer. Furthermore, recent studies demonstrate that ingested nitrate plays a role in host defence against gastrointestinal pathogenic bacteria. Analytical values of nitrate content in foods are essential for estimating nitrate intake. The analytical process is of paramount importance for assessing human nitrate exposure and for establishing a link between these exposures and the current and future observed health effects. Therefore, the quality assurance of the measurement process is crucial to obtaining reliability, comparability and traceability of results. Certified Reference Materials (CRM) should play a role in the consistency of the measurement process. However, the availability of nitrate CRMs is still poor. When food monitoring is demanded, an approach could be to use In House Reference Materials (IHRM), prepared at a high metrological level, and all preparation steps should be quality driven. IHRMs were prepared, and available CRMs were used to provide traceability of the process. The homogeneity of IHRM was evaluated using an appropriate statistical design. The stability was monitored using an isochronous method. The material shelf life and storage conditions are presented.HPLC was optimised for the determination of nitrates in four vegetable categories. When a suite of IHRMs were used, the response of the HPLC system was linear over the range 1 to 8 mg L^–1. The detection limit for these compounds was 0.2 g L^–1 and the determination limit 1.2 g L^–1.The relationship between measurement uncertainty and critical points of the analytical process is presented. The differences in observed relative uncertainty between food categories could reflect current limitations in the food matrix reference materials.