Comparison of sample preparation methods for the ICP-AES determination of minor and major elements in clarified apple juices

Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for the determination of minor and major elements present in apple juices. Prior to ICP-AES measurement, samples were diluted with nitric acid or digested in a microwave assisted digestion system. The differences in the measured element concentrations after application of different types of sample preparation procedures are discussed. The direct measurement compared to closed microwave dissolution was found to be the best sample preparation procedure. Prior to the measurements the ICP-AES method was validated and optimized for the determination of elements in apple juices. For diluted apple juice samples the lowest limits of detection (LOD) were obtained for Ba and Cd (< 20 μg L^{− 1}), moderate ones for Cu, Mn, Ni, Fe, Ag, Ca, Cr, Zn, Mg, and Sr (20–100 μg L^{− 1}), and the highest LODs for K, Pb, Na, and Al (> 110 μg L^{− 1}). The results obtained for the repeatability (< 0.9%), the intermediate precision (< 4.5%), the day-to-day reproducibility (< 5.2%), and the overall uncertainty of measurement (approx. 4–7%) for all elements analyzed demonstrated the good applicability of the proposed method. Differences in major element content in fresh and commercial apple juice are discussed.     

青海枸杞子中微量元素含量的测定

测定了青海枸杞子中锌、铜、锰、铅、砷、铁、硒等微量元素的含量。结果表明,青海枸杞子中含锌18.65μg/g,铜15.62μg/g,锰6.24μg/g,铅1.03μg/g,砷0.24μg/g,铁19.68μg/g,硒2.15μg/g,人体必需微量元素含量丰富,是枸杞具有极为重要的保健、防病、治病功能的重要原因之一。     

Ultra Sensitive Quantification of Thiourea at Nanomolar Level by Catalytic‐Kinetic Differential Pulse Voltammetry

A new simple and highly selective and sensitive catalytic differential pulse voltammetry procedure for the determination of thiourea at nanomolar level is reported. Thiourea has a catalytic effect on the oxidation of Janus green by iodate in the hydrochloric acid medium. The potential was scanned in the negative direction and the differential pulse voltammograms were recorded. The variations of the peak current with hydrochloric acid concentration, oxidant, Janus green, pulse amplitude, pulse time and scan rate were optimized. Under the optimized conditions, the relationship between the peak current and concentration of thiourea was obtained. It is shown that the calibration curve is linear in the range of 0.01–6.00 µg/mL. The detection limit of the method was 0.005 µg/mL. The relative standard deviation for 6 replicate determinations of 0.01, 0.50 and 2.00 µg/mL is equal to 2.25%, 1.52% and 1.03%, respectively. The method was applied to the determination of thiourea in fruit juices with satisfactory results.     

Molecularly imprinted nanoparticles-based electrochemical sensor for determination of ultratrace parathion in real samples

Molecularly imprinted polymer nanoparticles (nano-MIP), containing parathion selective sites, were synthesized by using suspension polymerization in silicon oil and then used for carbon paste electrode preparation. The obtained electrode was applied as an electrochemical sensor for parathion determination in different fruit and vegetable samples. Different factors including electrode composition, conditions of parathion extraction in the electrode and electrochemical measurement conditions were evaluated and then optimized by using various techniques of screening and response surface experimental designs. Electrode response to parathion (Res₁) and its selectivity for parathion (Res₂) were the desired responses. These responses were optimized simultaneously. After optimization, a sensor with high selectivity and picomolar detection limit were obtained. It was shown that the sensor response to parathion concentration was linear in the concentration range of 0.05 to 150?nmol?L^?1. The detection limit of designed sensor was calculated equal to 0.02?nmol?L^?1. The developed determination method was properly used for ultra-trace level assay of parathion in different fruit and cabbage samples.     

罐装橙汁超高温瞬时灭菌的数值模拟研究

由于对橙汁的灭菌工艺没有进行精确的研究,在橙汁的实际生产中经常是使用过度灭菌来保证果汁灭菌的彻底。过度灭菌不但引起橙汁生产的能耗增加而且会导致橙汁的营养成分的损失。本文分析了果汁中常见的细菌,得出了灭菌结束时所需的最低温度;在此基础上利用数值模拟的方法对橙汁的超高温瞬时灭菌进行了计算。同时使用实验对CFD计算的结果进行了验证,误差在9.5%以内,表明CFD对橙汁的超高温灭菌的模拟是可行的。模拟得出了不同温度时的灭菌的最理想时间条件分别为:135℃(408 K),13 s;140℃(413K),12 s;145℃(418 K),12 s;150℃(423K),11 s。     

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.     

应用废弃果皮制备绿色钻井液添加剂的综合性实验

设计了应用废弃果皮制备绿色钻井液添加剂的综合性实验,评价其对钻井液性能的影响.该实验将油田化学理论基础与实验技术、现场实践相结合,能够提高学生的专业实验技能、分析和解决问题的能力,同时采用废弃果皮作为实验原料,可提高学生的环保意识,有助于将环保理念注入日后油田生产中.     

傅里叶变换红外光谱结合化学计量学鉴别预包装纯菠萝汁中外源糖

为了快速、准确鉴别预包装纯菠萝汁是否掺有外源性糖,采用傅里叶变换衰减全反射中红外光谱技术采集900～1 500 cm-1范围内不同批次的预包装纯菠萝汁样品和掺入甜菜糖浆、大米糖浆、木薯糖浆的菠萝汁掺假样品的中红外光谱共计234例,以线性判别分析和支持向量机分析为掺假鉴别模型的建模方法,比较了全波段谱图与通过主成分载荷系数分析选取特征波长图谱的两种掺假鉴别模型。研究表明,全波段图谱的线性判别分析和支持向量机分类模型对验证集的判断正确率均高于88%;选取8个特征波长之后,线性判别分析模型验证集判断正确率提高至96.15%,支持向量机模型验证集判断正确率提高至94.87%,且模型输入变量由312个减少到8个。利用傅里叶变换衰减全反射中红外光谱技术结合化学计量学方法选取特征波长后建立的模型可以较好的应用于预包装纯菠萝汁外源糖的鉴别。     

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.     

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.