超高效液相色谱-串联质谱法测定不同茶叶中草甘膦、氨甲基膦酸及草铵膦的残留

建立了超高效液相色谱-串联质谱同时快速测定不同茶叶中草甘膦、氨甲基膦酸及草铵膦的方法。样品用0.05 mol/L NaOH提取,并以HCl调节pH值,Oasis HLB小柱净化除杂,氯甲酸-9-芴基甲酯(FMOCCl)柱前衍生反应后,超高效液相色谱-串联质谱法测定。本方法在5~1000μg/L浓度范围内,不同茶叶基质中草甘膦、氨甲基膦酸、草铵膦线性关系良好(R2>0.99)。在0.1,0.4和4 mg/kg添加水平下,不同茶叶(绿茶、红茶、乌龙茶、普洱茶)中3种化合物回收率均介于72.1%~109.9%之间,相对标准偏差RSD在0.5%~9.8%之间(n=6),方法定量限(LOQ)在0.03~0.08 mg/kg之间(S/N=10)。本方法稳定,简便,灵敏,能够满足检测需求。     

Fluorescence quantification of tetracycline in the presence of quenching matrix effect by means of a four-way model

In this work, a four-way tensor is used to model the quenching effect in fluorescent measurements. By means of the analysis of excitation-emission matrices obtained in the determination of tetracycline in tea, which acts as quencher, it is shown as the impossibility to use a calibration, or an addition standard based on a three-way model. It is analysed the quencher multiplicative effect made on the tetracycline signal by means of an ANOVA. However, by arranging the experimental data in a four-way tensor, it is viable to perform a calibration based on the parallel factor analysis, PARAFAC, decomposition and a four-way partial least squares, 4-PLS, regression to quantify the tetracycline in the presence of the matrix quencher effect. 4-PLS calibration provides better results. In the range from 40 to 220 μg L⁻¹ gives an average of relative errors in absolute value equal to 8.02% in prediction (3.40% in calibration). The repeatability as standard deviation in this range is 5.08 μg L⁻¹ and the method is accurate, slope and intercept being statistically equal to 1 and 0, respectively when a regression calculated versus true concentration is performed. Moreover, it has a decision limit (CCα) of 13.87 μg L⁻¹ for a probability of false positive, α, equal to 0.05 and a capability of detection (CCβ) of 26.63 μg L⁻¹ (for probabilities of false positive, α, false negative, β, equals to 0.05).     

Separation of catechins and methylxanthines in tea samples by capillary electrochromatography

In this paper, the simultaneous separation of several polyphenols such as (+)‐catechin, (–)‐epicatechin, (–)‐epigallocatechin, theophylline, caffeine in green and black teas by capillary electrochromatography (CEC) was developed. Several experimental parameters such as stationary phase type, mobile phase composition, buffer and pH, inner diameter of the columns, sample injection, were evaluated to obtain the complete separation of the analysed compounds. Baseline resolution of the studied polyphenols was achieved within 30 min by using a capillary column (id 100 μm) packed with bidentate C₁₈ particles for 24.5 cm and a mobile phase composed of 5 mM ammonium acetate buffer pH 4 with H₂O/ACN (80:20, v/v). The applied voltage and the temperature were set at 30 kV and 20°C. Precision, detection and quantification limits, linearity, and accuracy were investigated. A good linearity (R² > 0.9992) was achieved over a concentration working range of 2–100 μg/mL for all the analytes. LOD and LOQ were 1 and 2 μg/mL, respectively, for all studied compounds. The CEC method was applied to the analysis of those polyphenols in green and black tea samples after an extraction procedure. Good recovery data from accuracy studies ranged between 90% and 112% for all analytes.     

SPME-GC-MS分析瀑布毛峰茶叶的赋香成分

采用顶空-固相微萃取法(SPME)从瀑布毛峰茶叶中提取挥发性成分,用气相色谱-质谱法(GC-MS)分析其组成。从一级和特级茶叶中分别鉴定了相对含量大于0.50%的化合物48个和41个,其中共同组分27个。一级瀑布毛峰茶叶的主要挥发性成分有壬醛(9.22%),芳樟醇(4.75%),牛儿醇(4.07%),(Z)-3-己烯-1-醇(3.53%),十一醛(3.16%),邻苯二甲酸二异丁酯(2.94%),十六烷(2.35%),己醛(2.00%),1-辛醇(1.97%),6-甲基-5-庚烯-2-酮(1.86%)。特级瀑布毛峰茶叶的主要挥发性成分有:壬醛(8.85%),1-辛烯-3-醇(6.37%),十一醛(4.81%),2,5,5-三甲基-1-己烯(2.84%),辛醛(2.73%),1-辛醇(2.63%),6-甲基-5-庚烯-2-酮(2.60%),芳樟醇(2.20%),1-戊醇(2.20%),己醛(2.16%)。两个等级的瀑布毛峰茶的主要挥发性成分大致相同,但各成分的含量存在一定差异。     

单缝石英管火焰原子吸收法测定蒜头、茶叶、大米中微量硒

本法利用单缝石英管，提高火焰原子吸收法的灵敏度并降低测试成本。方法用于大米、蒜头、茶叶中硒的测定，获得满意的结果。     

火焰原子吸收光谱法连续测定茶叶中的钙镁

本文用火焰原子吸收光谱法连续测定茶叶中的钙、镁。方法简单、快速,具有良好的精密度和准确度,相对标准偏差１．８７％～２．７５％,回收率９２．５％～１０５．１％。     

分光光度法测定茶叶中的茶氨酸

热水萃取茶氨酸,浓盐酸水解为乙胺,建立了分光光度测定茶叶中茶氨酸含量的新方法。最大吸收波长为570nm。茶氨酸浓度在1.6-10.0mg·L-1范围内与△A呈线性关系,检出限为3×10-7g·mL-1。方法分析结果准确、操作比较简单、可排除茶叶中其它氨基酸的干扰。直接测定茶叶样品中的茶氨酸获得了满意的结果。     

原子吸收光谱法测定茶叶中的镁

镁是机体必不可缺的元素。采用原子吸收光度法对我国一些常见茶叶中的镁进行了测定 ,镁含量为1.2 9— 2 .0 7(mg/kg) ,茶汤中镁的浸出率在 14 .2— 5 1.8%。与一般食物相比 ,茶叶中镁含量更丰富 ,因此饮茶可延年益寿。     

Adsorptive Stripping Voltammetric Detection of Tea Polyphenols at Multiwalled Carbon Nanotubes‐Chitosan Composite Electrode

This study reports the catalytic oxidation and detection of tea polyphenols (TPs) at glassy‐carbon electrode modified with multiwalled carbon nanotubes‐chitosan (MWCNTs‐CS) film. The adsorption of TPs at the surface of the MWCNTs through π–π conjugation prevents the aggregation of nanotubes and induces a stable MWCNTs suspension in water over 30 days. Based on the adsorptive accumulation of polyphenols at MWCNTs, TPs is sensitively and selectively detected by adsorptive stripping voltammetry. The accumulation conditions and pH effect on the adsorptive stripping detection were examined. The linear range was found to be 100 to 1000 mg L^?1 with a detection limit of 10 mg L^?1 (S/N=3) for 2.5 min accumulation. Additionally, the MWCNTs‐CS electrode is easily renewed by applying positive potential to remove the adsorbed TPs. This method was successfully applied to determine TPs in commercially available teas with satisfied result compared with that of conventional spectrometric analysis.     

以热力学和动力学性质差异连续高敏测定磷和砷及其比较研究

提出以非离子表面活性剂使磷钼酸、砷钼酸－孔雀绿缔合物在水相增敏、增溶、增稳并根据磷（Ⅴ）、砷（Ⅴ）的氧化性差异及形成上述缔合物速率差异，分别建立了以热力学和动力学性质差异在水相不经分离、连续、简便、高敏测两组分的光度法，并对此两法进行了比较研究。摩尔吸光系数ε６５０分别为１．１１×１０５（磷）和１．２２×１０５（砷）Ｌ·ｍｏｌ－１·ｃｍ－１；服从比尔定律的浓度范围相应为０～０．２４和０～０．４８μｇ／ｍＬ。已成功地用于测定四种钢样（相对误差：热力学法皆不大于±５％，动力学法通常皆不大于±１０％）和两种茶样（回收率：热力学法为９８～１０２％，动力学法为９３～１１１％）。