Determination of tryptophan in feedstuffs: Comparison of two methods of hydrolysis prior to HPLC analysis

The tryptophan content of nine samples of commercial feed was determined using two procedures (I and II) differing mainly in the hydrolysis conditions used prior to analysis. With I, hydrolysis was performed with 4 M LiOH in the presence of maltodextrin with 5-methyltryptophan used as internal standard at 110°C for 24 h; with II. oxygen-free 1.3 M Ba(OH)₂ was used at 125°C for 16 h. The two procedures gave identical results for a given sample indicating that the corrections for the incomplete recovery of tryptophan 5-methyltryptophan quantitation were satisfactory.     

New HPLC Method to Determine Ethyl Carbamate in Alcoholic Beverages Using Fluorescence Detection

ABSTRACT: A new methodology to the quantification of ethyl carbamate (EC) has been developed. This method allows the analysis by HPLC of ethyl carbamate in samples of wine, fortified wine, and wine brandy, by a pre-column derivatization with 9-xanthydrol, and fluorescence detection. This does not require previous sample extraction or concentration. The method presents an average recovery of 96% among samples studied, a detection limit of 4.2μg/L, and an average intermediate precision of 6.3%. The comparison of the results obtained for EC analysis on the same wine brandy samples by GC/MS and HPLC are statistically indistinguishable with 97.5% probability. The results of the analysis of 42 samples are presented.     

液相色谱法测定萘普生中间体1-(6-甲氧基-2-萘基)乙醇

建立了萘普生中间体 1 (6 甲氧基 2 萘基 )乙醇的高效液相色谱分析方法。流动相 :甲醇 +水 =80 + 2 0 (v/v ) ,在C18柱上UV 2 38nm下测定其含量 ,方法精密度为 0 19,变异系数为 0 2 7% ,回收率在 98 5 %～ 10 0 4 %之间     

Selective recognition in molecularly imprinted polymer and its chromatographic characterization for cinchonine

A molecularly imprinting polymer (MIP) was synthesized via bulk polymerization under different conditions using anti-ague drug cinchonine (CN) as template. Infrared spectra (IR) results show that the template CNand functional monomer α-methyl acrylic acid (MAA) formed complexes before polymerization and the structure of complexes was simulated by Hyperchem. The results indicate that there are hydrogen bond or ionic bond between functional monomer and template molecule in acetonitrile solution. The MIP made in cold-initiated photo-polymerization has higher separation performance than that in the therm-initiated polymerization. The separation of the isomers CN and cinchonidine (CD) can be successfully obtained when its separate factor α reaches 1.82. Scatchard analysis suggests that the MIP recognizing CN with two classes of binding sites. The partition coefficient Kd, 1 and apparent maximum number nmax, 1 of binding sites with high affinity are 131.43 μmol/L and 58. 90 μmol/g, respectively,while Kd, 2 and nmax, 2 of binding sites with low affinity are 2.32 mmol/L and 169.08 mmol/g, respectively.     

Strawberry juice colour: The effect of some processing variables on the stability of anthocyanins

The colour stability of juice and purées made from a mixture of two strawberry varieties, stored at + 20°C or at –20°C under aerobic and anaerobic conditions, was studied. High-performance liquid chromatography and spectrophotometric analysis were used to monitor the changes in colour during storage. Pelargonidin 3-glucoside comprised 80% of the total anthocyanin content. Four other pelargonidin-based peaks were found, being 10.4%, 3.5%, 0.7% and 0.3% of the total and two cyanidin peaks were present, being 3.3% and 0.4% of the total. Clarification before storage caused considerable losses in the initial anthocyanin concentrations. Storage conditions (air versus nitrogen) did not influence the rate of loss of anthocyanins during storage or the formation of polymeric pigments. There were no losses in anthocyanins and no increase in the amount of colour measured at 510 nm due to polymers in samples stored at–20°C. Polymerisation occurred in the samples stored at + 20°C, especially in the clarified samples.     

Lutein and lutein esters in marigold flowers by high performance chromatography

Lutein and lutein esters in marigold flowers was quantitatively determined by high performance chromatography (HPLC) with ODS-C18 column. A mixture of CH3CN-CH3OH-CH3COOCH2CH2 with volume ratio of 55:1:44 was used as mobile phase at a flow rate of 1.0mL/min and detection was carried out at 480 nm. The column temperature was about 20℃. The contents of lutein and lutein esters were determined by analytical curve of lutein since lutein and lutein esters have the same spectral characteristics. Determination results of hexane extracts and saponified samples of lutein show that the saponification transforms the esters into free lutein. The increase of the content of dipalmitate and palmitate stearate reveals that the reaction includes transesterifications.     

Simultaneous HPLC quantification of total cholesterol,tocopherols and β-carotene in Barrosã-PDO veal

A simple, rapid and sensitive procedure for the simultaneous determination of total cholesterol, tocopherols and β-carotene in meat is described. The method involves a direct saponification of the meat, a single n-hexane extraction and the analysis of the extracted compounds by normal-phase HPLC, using fluorescence (tocopherols) and UV–Vis photodiode array (cholesterol and β-carotene) detections in tandem. Rates of recovery of spiked meat samples were 93% for cholesterol, 83–86% for (α-, β- and -γ) tocopherols and 89% for β-carotene. Repeatabilities were high (CV < 6%) for all determined compounds, except for δ-tocopherol. This tocopherol, which is not usually present in meat, showed a much lower recovery percentage (73%) and repeatability (12.8%). This methodology was applied for the quantification of total cholesterol, tocopherols and β-carotene in three muscles (longissimus thoracis, longissimus lumborum and semitendinosus) of the Portuguese traditional Barrosã-PDO veal, obtained from autochthonous calves fed extensively during summer (with the least abundant green pastures) and slaughtered in early autumn (October). Barrosã-PDO veal showed median contents of total cholesterol (0.50–0.56 mg/g) and, depending on the analysed muscle, moderate to high contents of α-tocopherol (3.3–3.9 μg/g) and β-carotene (0.07–0.09 μg/g), suggesting an high sensorial and hygienic quality.     

Anthocyanins characterization of 15 Iranian pomegranate (Punica granatum L.) varieties and their variation after cold storage and pasteurization

Anthocyanins (ACs) are phenolic compounds that are distributed widely in fruits and vegetables. Apart from imparting color to plants, ACs also have an array of health-promoting benefits. In this research, the amounts of major ACs of 15 pomegranate (Punica granatum L.) varieties obtained from Yazd province were determined. The major ACs detected in the studied varieties were as follows: delphinidin 3-glucoside (2.19–16.29 mg/L), delphinidin 3,5-diglucoside (2.36–63.07 mg/L), pelargonidin 3-glucoside (0.26–1.36 mg/L), pelargonidin 3,5-diglucoside (0.01–8.11 mg/L), cyanidin 3-glucoside (5.78–30.38 mg/L), and cyanidin 3,5-diglucoside (4.39–166.32 mg/L). The effect of storage time of unprocessed and pasteurized juices on ACs content of four selected varieties was also studied. Average degradation percentage of each AC was between 23.0 and 83.0% during 10 days at 4 °C. Moreover, in pasteurized juices average degradation of ACs was 42.8 ± 0.5% after 10 weeks storage at 4 °C.     

用HPLC法测定对二异丙苯的一氢过氧化物和二氢过氧化物

二过氧化氢对二异丙苯是二异丙苯氧化法生产对苯二酚的重要中间产物。本文用HPLC半制备柱制得一过氧化氢对二异丙苯和二过氧化氢对二异丙苯纯品,用光谱法确定其结构,建立了正相高效液相色谱测定方法。     

双参数Bézier曲线的升二次扩展

本文以二次Bernstein基函数为例,首次提出了含双参数基函数的新扩展——αβQ—Bern-stein基函数,此类基函数具有新的特点,即基函数的扩展次数一次性升高两次,且包含了二次多项式和带一个参数的三次多项式基函数的所有性质。基于这组基函数定义了αβQ—Bézier曲线,该曲线也含有参数,具有形状可调性,当α与β取某些值时曲线能达到C4连续或在某个端点处C0连续。最后与含两个参数的升一次Bézier曲线进行比较,该曲线具有调节范围广、灵活性更强的优势。