新型3D纸基微流控分析器件的研制及应用

基于棉涤线进样通道、过滤区、检测区和"开关元件",研制了一种新型3D纸基微流控分析器件,并应用于食盐中IO-3的测定。实验探讨并优化了该器件的制备和测定条件。在优化的测定条件下,显色测定灰度值与IO-3浓度在5~250μmol/L范围内呈线性关系,检出限为2.3μmol/L。该方法可应用于实际样品中IO-3的测定。     

酸性品红褪色光度法直接测定食盐中的碘

在HCl-KBr的介质中,碘酸钾氧化酸性品红褪色的程度与碘酸根含量在一定范围内呈线性关系,从而建立了褪色光度法测定碘的新方法。试验结果表明,酸性品红的最大吸收波长为545nm,碘的含量在0.4—2μg·mL-1范围内时,符合比耳定律,表观摩尔吸光系数为3.7×104L·mol-1·cm-1。用于测定食盐中的碘,结果满意。     

Inductively coupled plasma atomic emission spectrometric determination of 27 trace elements in table salts after coprecipitation with indium phosphate

The coprecipitation method using indium phosphate as a new coprecipitant has been developed for the separation of trace elements in table salts prior to their determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). Indium phosphate could quantitatively coprecipitate 27 trace elements, namely, Be, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Pb, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, in a table salt solution at pH 10. The rapid coprecipitation technique, in which complete recovery of the precipitate was not required in the precipitate-separation process, was completely applicable, and, therefore, the operation for the coprecipitation was quite simple. The coprecipitated elements could be determined accurately and precisely by ICP-AES using indium as an internal standard element after dissolution of the precipitate with 5 mL of 1 mol L⁻¹ nitric acid. The detection limits (three times the standard deviation of the blank values, n = 10) ranged from 0.001 μg (Lu) to 0.11 μg (Zn) in 300 mL of a 10% (w/v) table salt solution. The method proposed here could be applied to the analyses of commercially available table salts.     

Characterization of must and wine of six varieties of grapes by direct infusion electrospray ionization mass spectrometry

Samples of must derived from six different varieties of grapes taken during the fermentation process, as well as the respective wine samples directly after the end of the malolactic fermentation, were analyzed by direct infusion negative ion mode electrospray ionization mass spectrometry (ESI-MS). Diagnostic ions for must were different from those of wine samples, although small variations for each of the grape varieties were also detected. The addition of unfermented must or sugar to wine could also be clearly detected. The spectra were acquired in a few minutes per sample, indicating that ESI-MS can be used for high-throughput analysis of samples and should prove useful for quality control during and after the fermentation process.     

基于离子交换-电导检测法对酿酒葡萄中有机酸含量进行分析

建立了离子色谱法测定酿酒葡萄中乳酸、丙酸、苹果酸、酒石酸、草酸、柠檬酸、琥珀酸和抗坏血酸的方法。样品经提取、脱色、过滤后以自动淋洗液发生器生成的1.5~30 mmol/L KOH为淋洗液洗脱,抑制电导检测器检测。考察了共存非测定离子及相邻离子间的干扰,结果表明非测定无机离子对测定无干扰。8种有机酸在一定浓度范围内与其峰面积呈良好的线性关系,检出限为0.064~0.25 mg/L,加标回收率为89.5%~96.2%。该方法用于宁夏贺兰山东麓酿酒葡萄中8种有机酸分析,8种有机酸均被检出,以苹果酸和酒石酸含量最高,柠檬酸次之,其它酸含量均较低。酿酒葡萄为典型的酒石酸型水果。     

停流流动注射-化学发光法测定碘盐中的碘酸根

基于在酸性介质中 ,IO-3 与 I-快速反应产生 I2 ,I2 氧化 Luminol产生化学发光反应的机理 ,建立了Luminol- IO-3 偶合发光体系测定微量 IO-3 的方法。本法测定 IO-3 的线性范围为 5 .0× 10 -8- 3.0× 10 -5g/m L;检出限为 5 .0× 10 -8g/m L ;该法中的采样、停流和进样都由计算机自动控制 ,操作简便 ,灵敏度高 ,选择性好。应用于含碘食盐中微量 IO-3 的测定 ,结果令人满意     

结晶紫选择电极的制备及催化电位法测定碘的研究

根据磷酸介质中碘离子催化高碘酸钠氧化结晶紫的氧化还原反应,应用自制的结晶紫选择电极跟踪紫的 度变化,对催化电位法测定碘进行了研究。测定碘离子 的线性范围为０．２０－５．５μｇ／２５ｍＬ,方法检出限为４．１＊１０＾－９ｇ／ｍＬ。该方法应用于测定食盐和饮用水中碘含量,ＲＳＤ〈４．１％,平均回收率为９５．１％。     

Conditions for Homogeneity of Subpopulations

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氢化物发生/原子吸收分光光度法测定食盐中铅

采用氢化物／原子吸收光谱法测定食盐中痕量铅，使用流动注射氢化物发生器，自动吸入试样和NaBH4溶液，空气／乙炔火焰加热石英管原子化器。对测定条件及共存元素的允许量进行了研究，采用K3[Fe(CN)6]作氧化剂。方法的灵敏度是0．28n/mL/1％吸收，检出限为0．10ng/mL，回收率在94％－102％之间，RSD为2．1％－5．3％。     

倍增反应紫外吸光光度法测定食盐中微量碘

在硫酸介质中 ,IO-3 氧化I-产生 3倍摩尔量I-3 ,而I-3 在紫外光区的 2 88nm具有最大吸收 ,ε2 88=1.3×10 5L·mol-1·cm-1,具有很高的灵敏度 .碘的浓度在 0～ 6 0 μg/ 10 0mL范围内符合比耳定律 ,方法简便快速、选择性好、灵敏度高 ,用于测定加碘食盐中碘的含量 ,结果满意