膜富集固相萃取-漫反射光谱法快速测定食品中柠檬黄北大核心CSCD

色素作为食品中常用的添加剂,近年来受到广泛关注。人工合成色素通常较天然色素色彩鲜艳、坚牢度大、稳定性强、价格低廉,所以有着广泛的应用[1]。柠檬黄是人工合成黄色素中具有代表性的一种,其为橙黄色均匀粉末,可溶于水,耐热性、耐光性等均好,被广泛用于饮料、固体食品中,但柠檬黄分子中含有苯环等结构,具有毒性,食品中最大使用量为100 mg·L-1[2]。因此,检测饮料中柠檬黄十分重要。     

双水相体系选择性分离富集维生素B_(12)及电热原子吸收法测定

用异丙醇-硫酸铵双水相体系,利用维生素B12的疏水性和硫酸铵的盐析作用,在高浓度无机Co2+共存的情况下可有效地实现维生素B12的选择性分离富集.对双水相体系的组成、萃取时间和pH等实验参数进行了优化,在2.0mL样品、1.1g硫酸铵和200μL异丙醇组成的双水相体系中,对50μgL-1的维生素B12溶液经过萃取分离后富集倍数为11.8.取20μL双水相体系上相进行电热原子吸收检测,线性范围为2～100μgL-1,检出限为0.6μgL-1(3σ,n=11),相对标准偏差为2.8%(50μgL-1,n=9).将所建立的方法应用于功能饮料、保健药片、牛肝等实际样品中维生素B12的含量测定,加标回收率在97%～104%之间.     

吐温80-盐-水体系的液-固萃取光度法测定痕量钴

研究了Ｃｏ（Ⅱ）－ＰＡＲ在吐温８０－硫酸铵体系中的最佳萃取条件,建立了生物样品中测定痕量钴的非有机溶剂液－固萃取光度法。在ｐＨ７．０～１０．５的ＮＨ３．Ｈ２Ｏ－ＮＨ４Ｃｌ缓冲溶液中,１金属配合物Ｃｏ（Ⅱ）－ＰＡＲ可被吐温８０固相富集,最大吸收波长为５１５ｎｍ,钴含量在０～５．０ｕｇ／ｍＬ范围内服从比尔定律,可用于头发、茶叶和维生素Ｂ１２针剂中痕量钴的测定。     

极谱法测定维生素B12中的痕量钴

在pH 10,0.04 mol/L的NH3*H2O-NH4Cl缓冲溶液中,钴-百里香酚酞在NaNO2存在下,于-1.25 V(vs.SCE)产生一尖锐、灵敏的二次导数极谱波,峰电流与钴(Ⅱ)浓度在5.0×10-8～5.0×10-6 mol/L范围内呈线性关系,检出限为2.0×10-8 mol/L.研究了该波的性质,证明该波为吸附波.方法用于维生素B12中痕量钴的测定,结果满意.     

漫反射傅里叶变换红外光谱法测定维生素C制剂中抗坏血酸的含量

采用漫反射傅里叶变换红外光谱法(DRIFTS)测定维生素C制剂中抗坏血酸的含量。选择合适的分析峰1660~1680 cm–1,可排除其它成分的影响,吸光度与抗坏血酸的浓度呈良好线性关系。以镜面为背景,以75μm筛过筛后的KBr为稀释剂,用DRIFTS法分别测定了3种市售维生素C制剂中的抗坏血酸含量,测定结果分别为75.60%,9.80%,6.72%;相对标准偏差(n=6)分别为6.6%,4.9%,8.2%,与碘量法测定结果接近。样品加标回收率为94.0%。DRIFTS法测定维生素C中的抗坏血酸方法简便、准确,无试剂消耗,无废液产生,是非破坏和非污染的绿色分析方法。但其测定结果的精密度不如碘量法,而且其测定结果的准确程度受样品的性状限制,对于白色粉末或可研磨为粉末的样品分析结果准确度较高。     

阻抑动力学光度法测定维生素B_(12)中痕量钴(Ⅱ)

钴是人体必需微量元素,是维生素B_(12)的一种极其重要的组成成分,当维生素B_(12)及钴缺乏时,核酸合成受阻,可发生巨幼红细胞性贫血,临床叫恶性贫血,因此,研究钴的高灵敏分析方法具有重要的意义。催化动力学光度法具有灵敏度高、选择性好,设备简单、操作简便的特点,是测定痕量钴的有效方法之一。在钴的催化动力学分析中,报道较多的是依据钴(Ⅱ)对反应的加速即正催化,对阻抑催化     

钴(Ⅱ)-茜素红-罗丹明B-聚乙烯醇体系光度法测定痕量钴

提出了钴 (Ⅱ ) 茜素红 罗丹明B 聚乙烯醇体系光度法测定钴 (Ⅱ )的新方法。该方法灵敏度高 ,ε =3.2 8× 10 5L·mol- 1·cm- 1,线性范围为 0～ 7.5 μg/ 5 0ml,测定 2 μg钴 (Ⅱ ) 6次 ,RSD为2 .6 6 % ,用于水中痕量钴的测定 ,结果满意     

双分子维生素B_(12)模型分子的合成及表征

维生素B_(12)经醇解得到的七甲基钴啉酯1作为起始原料，经酸性水解分别得 到b,c,d,e,f-单酸钴啉酯2b～2f, 2b～2f与3-咪唑基丙胺盐酸盐反应合成了相应的 酰胺钴啉酯衍生物3b～3f, 3b～3f在乙酸的作用下合成了双分子络合维生素B_(12) 模型化合物双-单腈六甲基-N-（3-咪唑基）丙酰胺钴啉酯高氯酸盐5b～5f，并对其 化学结构进行了表征。     

自然水、维生素B_(12)和人眼泪中痕量钴的测定

极谱催化波测定钴,以前大多采用丁二肟和其他含氮有机试剂为配位体进行测定。但这类体系需在碱性溶液中进行,而且催化波出现在较负的电位,影响了实际应用。我们发现在3,5-二溴-PADAP-NaNO_2的弱酸性介质中,钴产生一个灵敏的极谱波,继后又发现用5-Cl-PADAB代替3,5-二溴-PADAP可进一步提高灵敏度,而且络合物的峰电位与试剂的峰电     

膜富集-紫外光谱法快速检测自来水中痕量2-萘酚

基于紫外光谱结合膜富集技术,提出了一种快速、灵敏检测自来水中2-萘酚的方法。以尼龙滤膜(孔径0.22μm)为富集材料,将富集到膜上的2-萘酚不经洗脱直接测定其漫反射紫外光谱,以实现定量分析目的。该方法方便快捷,大大提高了灵敏度。对p H值、样品体积和真空度等条件进行优化,并对方法的分析性能进行了评价。结果显示,2-萘酚的浓度与吸光度(波长为331 nm)在0.3~10 mg/L范围内用二次函数可得到良好的拟合关系,在0.3~1.0 mg/L和1.0~10 mg/L范围内呈分段的线性关系,相关系数(r2)分别为0.999 1和0.995 5。在最佳条件下,检出限达0.265 6 mg/L。该方法准确度和精密度较理想,适用于对自来水中2-萘酚的检测。     

近红外光谱结合膜富集技术测定饮料中微量邻苯二甲酸二异辛酯的含量

提出了一种基于在线膜富集的近红外漫反射光谱技术,对饮料中的微量塑化剂邻苯二甲酸二异辛酯(DEHP)进行快速检测。采用聚醚砜膜对饮料中的DEHP进行富集,将富集DEHP的膜直接进行近红外漫反射检测。参考DEHP的透射近红外光谱,对波数进行选择,以4 420～4 060、4 700～4 540、6 040～5 600cm-1作为建模的波数区间。通过比较原始光谱、多元散射校正、一阶求导、二阶求导及其组合,考察了光谱预处理方法对模型的影响,用去一交互验证法建立了偏最小二乘(PLS)模型,并用所建立的校正模型对校正集样品进行了预测。结果表明,在选定的波数区间,当用一阶求导对校正集光谱进行预处理时,所建立的模型对校正集的预测效果最佳,在隐变量数为7时,对校正集所有样品的校正均方根误差(RMSEC)为0.188 7mg/L。用此模型对预测集样品进行预测时,DEHP的质量浓度在0.5～5.0 mg/L范围内,预测均方根误差(RMSEP)为0.232 4 mg/L,平均相对预测误差为6.29%。     

Application of Near Infrared Diffuse Reflectance Spectroscopy with Radial Basis Function Neural Network to Determination of Rifampincin Isoniazid and Pyrazinamide Tablets

Partial least squares(PLS),back-propagation neural network(BPNN)and radial basis function neural network(RBFNN)were respectively used for estalishing quantative analysis models with near infrared(NIR)diffuse reflectance spectra for determining the contents of rifampincin(RMP),isoniazid(INH)and pyrazinamide(PZA)in rifampicin isoniazid and pyrazinamide tablets.Savitzky-Golay smoothing,first derivative,second derivative,fast Fourier transform(FFT)and standard normal variate(SNV)transformation methods were applied to pretreating raw NIR diffuse reflectance spectra.The raw and pretreated spectra were divided into several regions,depending on the average spectrum and RSD spectrum.Principal component analysis(PCA)method was used for analyzing the raw and pretreated spectra in different regions in order to reduce the dimensions of input data.The optimum spectral regions and the models' parameters were chosen by comparing the root mean square error of cross-validation(RMSECV)values which were obtained by leave-one-out cross-validation method.The RMSECV values of the RBFNN models for determining the contents of RMP,INH and PZA were 0.00288,0.00226 and 0.00341,respectively.Using these models for predicting the contents of INH,RMP and PZA in prediction set,the RMSEP values were 0.00266,0.00227 and 0.00411,respectively.These results are better than those obtained from PLS models and BPNN models.With additional advantages of fast calculation speed and less dependence on the initial conditions,RBFNN is a suitable tool to model complex systems.     

Determination of Vitamin B12 in Multivitamin Tablets by High Performance Liquid Chromatography

Abstract

Two procedures for separation and determination of vitamin B₁₂ in multivitamin tablets by reversed phase high performance liquid chromatography are proposed. Sample preparation is very simple: tablets are dissolved in distilled water, centrifuged and filtered. The sample solution is directly applied in the sample loop injector and chromatograms are obtained with gradient elution using water-methanol and water-acetonitrile as solvents. The peak of vitamin B₁₂ from samples of B-complex tablets is well separated with the two procedures. For multivitamin tablets, however, only the procedure with water and methanol as solvents was good for separation and quantification of vitamin B₁₂. Both procedures were verified by the standard addition method and also compared to a previously developed method using electrothermal atomic absorption spectrometry for vitamin B₁₂ determination.     

Speciation of Chromium in Natural Waters,Tea, and Soil with Membrane Filtration Flame Atomic Absorption Spectrometry

A sensitive and selective method was developed for the speciation of chromium(III) and chromium(VI) in environmental samples based on membrane filtration and determination by flame atomic absorption spectrometry. Chromium(III) reacts with cochineal red A, yielding a complex that is adsorbed on a cellulose acetate membrane filter, whereas chromium(VI) remains in aqueous solution, permitting separation. After reduction of chromium(VI) to chromium(III) with hydroxylamine hydrochloride, the total concentration of chromium was determined, and the concentration of chromium(VI) was calculated by subtraction. The pH, amount of cochineal red A, and sample volume were optimized on the basis of the recovery of Cr(III). The influence of matrix ions was also investigated. The preconcentration factor was 94. The detection limit (3 sigma) for Cr(III) was 1.4 micrograms per liter. The method was validated using environmental certified reference materials. The method was successfully employed for the speciation of chromium in wastewater and lake water.     

PVC-PP树脂分离富集/火焰原子吸收光谱法测定海水中痕量铜镍钴

采用自制的聚氯乙烯多乙烯多胺（PVC-PP）树脂,在pH值为5．0的条件下,分离富集海水中的痕量铜、镍、钴,以1．2mol／L盐酸溶液洗脱．火焰原子吸收光潜法测定,富集倍数最大可达100倍（回收率大于90％）。研究了吸附与洗脱的最佳条件,方法检出限分别为铜0．81μg/L、镍0．98μg/L、钴0．57μg/L（富集倍数100,S／N=3）,相对标准偏差小于5％（n=7）,样品加标回收率在90％-105％之间。     

超高效液相色谱串联质谱法测定婴儿奶粉中的维生素B_(12)

建立了超高效液相色谱串联质谱法测定婴儿奶粉中维生素B12的方法。采用三氯乙酸沉淀蛋白质,HLB固相小柱吸附净化提取液中的维生素B12,以50%的甲醇洗脱,吹去甲醇后定容测定,色谱柱为ACQUTITY UPLC BEH C18柱,以甲醇–10 mmol/L乙酸铵水溶液为流动相梯度洗脱,MRM模式,定量离子为m/z 678.3/147.2。在优化条件下,线性范围为0.5~200μg/L,相关系数(r)为0.999 3,检出限为0.3μg/kg,回收率为88.3%~92.9%,测定结果的相对标准偏差小于5%(n=6)。方法具有样品处理简单、灵敏度高、重现性好、分析时间短等优点,可以作为实验室常规测定婴幼儿奶粉中维生素B12的方法。     

正交实验优化的氢化物发生原子荧光法测定水中痕量锑

采用盐酸为介质,以顺序注射-氢化物发生原子荧光法测定生产用水中的锑含量．通过正交实验确定了仪器工作参数,研究了介质浓度、KBH4浓度、硫脲一抗坏血酸加入量等因素对测定结果的影响,探讨了共存离子的干扰．在选定的最佳实验条件下,方法的检出限为0．011ng/mL,线性范围0～8ng／mL,相对标准偏差为2．78％～6．20％,加标回收率为91．0％～99．1％．该方法操作简便,灵敏度高,准确度好,与微波消解法相比较,两者无显著性差异．