配糖蛋白B—阳离子丙烯酸树脂微胶囊的性能研究

本文研究了配糖蛋白B-阳离子丙烯酸树脂微胶囊的形态、粒径及粒径分布,并在模拟胃液的酸性缓冲液中进行了微胶囊的溶解释放试验。结果表明该微胶囊能溶于人体的胃液中,可配制适合儿童口服的混悬剂。     

改性生物凝胶对重金属离子的吸附性能研究

以桔子汁加工残渣为原料,制备钙型和氢型生物凝胶作为吸附剂,用于去除水溶液中的重金属离子.结果表明,上述凝胶在水溶液中稳定性较好,对重金属离子的吸附性能优良.钙型凝胶的吸附选择性顺序为:Fe3 ＞Pb2 ＞Cd2 ＞Zn2 ,饱和吸附容量分别为:Pb2 、Cd2 、Zn2 均为约1.1mmol/g、Fe3 为1.5mmol/g;氢型凝胶的吸附选择性顺序为:Pb2 ＞Zn2 ＞Cd2 .钙型凝胶对Fe3 的吸附行为明显不同于氢型凝胶,钙型凝胶以离子交换机理以及Fe3 与Ca2 之间的共沉淀作用为主;而氢型凝胶对Fe3 的吸附则以离子交换机理为主.     

Method validation for direct determination of some trace and toxic elements in soft drinks by inductively coupled plasma mass spectrometry

The consumption of soft drink beverages has increased in the last few years around the world and it is related to the diversity of brands and flavours available, increasing also the risk of ingestion of compounds considered non-beneficial to the health of consumers. In this study, fast, easy and simple method of analysis for direct determination of As, Pb, Cd, Sb, Hg, Cu, Zn, Fe, Al, Cr, Sn, Co, Mn and Ni in soft drink samples using quadrupole inductively coupled plasma mass spectrometry (Q-ICP–MS) was validated. The estimated detection limits, practical quantification limits, linearity (linear dynamic ranges and method linearity), accuracy (trueness and precision) and measurement uncertainty parameters were studied under optimised (Q-ICP–MS) conditions. The method showed that the estimated detection limits were varied between 0.02 and 2.403 µg/L, and the quantification limits were varied between 0.5 and 20 µg/L. The mean recoveries ± standard deviations at different spiking levels were varied between 75.03 ± 0.62% and 117.07 ± 2.83% and the coefficients of variation were varied between 0.49% and 9.79%. The method trueness was confirmed by using four different certified reference materials (soft drinks and treated water) purchased from FAPAS (Food Analysis Performance Assessment Scheme) and all obtained results were within satisfactory ranges and had acceptable recovery and Z-score values. The method precision, in terms of relative standard deviation, was below 4.88%. The method uncertainty expressed as expanded uncertainty of all validated elements was found to be ≤22.52%. The results obtained make the method suitable for accurate determination of validated elements in different kinds of soft drink samples at these low concentration values. Validated method was used for the determination of metallic contaminants in 40 commercial soft drink samples and the results were compared with the provisional guideline of the elements stated by Egyptian, WHO and European standards in drinking and potable bottled natural mineral water.     

A rapid and sensitive reversed phase‐HPLC method for simultaneous determination of ibuprofen and paracetamol in drug samples and their behaviors in simulated gastric conditions

Paracetamol is a widely used drug for fever and pain relief. Ibuprofen is a common nonsteroidal anti‐inflammatory drug. In this study, a sensitive and accurate reversed phase high performance liquid chromatography method was developed for the simultaneous determination of ibuprofen and paracetamol. The chromatographic separation was achieved on a Phenomenex C18 (250 mm, 4.6 mm, 5 μm) column. Fifty milli molar phosphate buffer (pH 7.5) and methanol were used as mobile phase in a gradient elution mode. The retention times of paracetamol and ibuprofen were 5.7 and 10.4 min, respectively. The linearity of the developed method was established in the range of 0.25 – 250 mg/L with a correlation coefficient of 0.9998 for both analytes. The limit of detection/quantification values were found to be 0.06/0.19 and 0.08/0.26 mg/L for ibuprofen and paracetamol, respectively. The method was successfully applied in drug samples in the form of tablets and suspensions. The calculated concentrations matched with the claimed values on their prospectuses. The drug samples were studied under simulated gastric conditions to determine the behaviors of the analytes in the human body. The obtained results showed no change in the retention time of the analyte peak shapes throughout the 210 minutes.     

Development and application of SBA‐15 assisted electromembrane extraction followed by corona discharge ion mobility spectrometry for the determination of Thiabendazole in fruit juice samples

A new sample preparation method based on SBA‐15 assisted electromembrane extraction coupled with corona discharge ion mobility spectrometer was developed for the determination of Thiabendazole as a model basic pesticide in fruit juice samples. The addition of SBA‐15 in the supported liquid membrane in electromembrane extraction system not only can lead to enhancement of the effective surface area, but also introducing the negatively charged silanol groups into supported liquid membrane might improve migration of positively charged analytes toward the supported liquid membrane and finally into the acceptor solution. To investigate the effect of the presence of SBA‐15 in the supported liquid membrane on the extraction efficiency, a comparative study was carried out between the conventional electromembrane extraction and SBA‐15/electromembrane extraction methods. Under the optimized conditions, SBA‐15/electromembrane extraction method showed higher extraction efficiencies in comparison with conventional electromembrane extraction method. SBA‐15/electromembrane extraction method exhibited a low limit of detection (0.9 ng/mL), high preconcentration factor (167) and high recovery (83%). Finally, the applicability of SBA‐15/electromembrane extraction method was studied by the extraction and determination of Thiabendazole as a model basic pesticide in fruit juice samples.     

表面增强拉曼光谱法分析软饮料中的阿斯巴甜

应用超声技术辅助预处理,以纳米银为活性基底,在溶液pH 5.0、纳米银与阿斯巴甜(APM)混合比例1∶1、混合温度30℃、加热时间6 min的条件下,利用表面增强拉曼光谱(SERS)结合化学计量法对纯品及软饮料中APM进行定量检测。结果表明:APM在0.5～100 mg/L范围内线性关系较好,其中水标准溶液的相关系数为0.993 3,检出限(LOD)为0.41 mg/L,苏打水、雪碧、可乐、芬达等标准溶液的相关系数为0.974 7～0.984 8,加标平均回收率为88.4%～121%,相对标准偏差小于7%。运用SERS检测软饮料中APM具有分析速度快、无损、环境污染小等优点,适用于食品中阿斯巴甜的定量分析,为食品添加剂的进一步表征和检测建立了依据,显示了SERS技术在化学物质检测领域具有巨大潜力。     

Manothermosonication (MTS) treatment of apple-carrot juice blend for inactivation of Escherichia coli 0157:H7

This study was performed to evaluate the responses of Escherichia coli 0157:H7 inoculated in an apple-carrot blended juice to manothermosonication (MTS) treatments. The MTS treatments were conducted in a continuous-flow MTS system. The juice samples were exposed to ultrasound treatment at combinations of three temperatures (60, 50 and 40 °C) and three pressure levels (100, 200, and 300 kPa) for five residence times (15, 30, 45, 60, and 75 s). The results showed that higher treatment temperature (i.e. 60 °C) and hydrostatic pressure in the MTS system significantly enhanced the microbial reduction. A FDA mandated 5-log CFU/ml reduction of E. coli 0157:H7 for juice processing was achieved in 30 s for MTS treatment at 60 °C, in comparison to 60 s at 50 °C. The Weilbull and Log-logistic models provided the best fitting of the inactivation data for the MTS treatments. Extensive damage of E. coli 0157:H7 cells treated with MTS was observed on micro-images of scanning electron microscopy and transmission electron microscopy.     

气相色谱法测定果汁饮料中甜蜜素含量的不确定度评定

采用气相色谱法测定果汁饮料中甜蜜素的含量,对测定结果的不确定度进行了分析,对各不确定度分量进行了评定和量化,计算了合成标准不确定度和扩展不确定度。不确定度主要来自量器校准和标准曲线引入的不确定度。果汁饮料中甜蜜素的含量结果表示为（0．350±0．023）g／kg,k=2。     

稳定同位素比质谱法测定苹果和浓缩苹果汁的δ13C值

用从国际原子能机构溯源得到的橄榄油标准物质[Cat No.B 2172-Batch 3130,其δ13CPDB为(-28.51±0.16)‰]作标准,应用稳定同位素比质谱法测定了苹果和苹果汁的δ13 C值,并以此确定国产苹果的δ13 C值的范围和鉴定制成的果汁的质量。苹果样品去皮后切碎,打成糊状,离心后取其上清液,在75℃加热2～3h至呈黏稠状液体,冷却至室温。此时其糖度约为70Brix。浓缩苹果汁样品是黏稠液体,其糖度一般也在70Brix左右。取2μL上述样品置于锡杯中,按方法处理后供质谱分析。标准物质的进样量为2μL。按所测得碳的稳定同位素13C与12C的比值代入所给公式计算δ13 C值。结果表明:方法的精密度较好,其相对标准偏差(n=11)均小于0.021%。根据测定结果发现,我国苹果的δ13C值在-29.1‰～-23.33‰之间。     

黑莓汁及其发酵制品中鞣花酸的高效液相色谱测定

建立了高效液相色谱(HPLC)法测定黑莓汁及其发酵制品中鞣花酸含量的方法。采用Waters symmetry C18色谱柱(250×4.6 mm,5μm),流动相为体积比44∶2∶54的甲醇-乙酸乙酯-KH2PO4/H3PO4(5%)溶液(磷酸调pH为2.7),流速0.6 mL/min,检测波长:0～6 min 400 nm,6～7.5 min 350 nm,7.5～30 min 254 nm。该方法检测黑莓汁中鞣花酸含量,平均回收率为99.08%,相对标准偏差(RSD)为0.077%。同时采用此方法跟踪检测了黑莓发酵液中鞣花酸的含量。结果表明,黑莓汁样品无需经过复杂的前处理,即可达到良好的分离。方法操作简单,准确度高,无杂质干扰,可用于黑莓原汁及黑莓汁发酵制品中鞣花酸含量的测定。