高效液相色谱法测定头孢拉定制剂方法的改进

目的:改进头孢拉定制剂含量测定方法。方法:高效液相色谱条件:以Shim—Pack CLC—ODS(250mm×4.6mm)为色谱柱;柱温为35℃;流动相为水—甲醇—3.86％醋酸钠溶液-4％醋酸溶液(1364:500:30:6);流速为0.8mL·min~(-1);检测波长为254nm。结果:头孢拉定峰形良好,分离度和柱效满足药典要求,保留时间由原来的21.32min缩短至8.06min,提高了分析速度,含量测定结果与中国药典无显著差异。结论:该方法快速、准确、能更好地适用于常规检验工作和大批量生产时的质量控制。     

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.     

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.     

6-硝基-1,2-重氮氧基-4-萘磺酸及其杂质的高效液相色谱分析

本文以反相高效液相色谱对6-硝基-1，2-重氮氧基-4-茶磺酸及有机杂质进行了分析，选择了流动相、离子对、检测波长，研究了不同牌号ODS C18色谱柱的重现性，得到了6-硝基-1，2-重氮氧基-4-萘磺酸及杂质(1，2-重氮氧基-4-萘磺酸、8-硝基-1，2-重氮氧基-4-萘磺酸)的相关系数分别为：0.99956、0.99991、0.99317；标准偏差和变异系数分别为：0.214250％、0．016890％、0．564557％、0.012695%、0.488467％、0.014560％得到了准确度数据，确定了最小检出量。     

Enhanced extraction of isoflavones from Korean soybean by ultrasonic wave

The amounts of isoflavones extracted from Korean soybean by various ultrasonic waves were compared using 60% aqueous ethanol solution. The effect on extraction yield of variations in solvent composition, temperature, and extraction time was investigated. The experimental results confirmed that ultrasonic waves are a desirable method to extract isoflavones from Korean soybean. The highest yield of aglycone isoflavones was obtained by ultrasonic waves with a frequency of 20 KHz and an extraction time of 10 min, which produced yields of glycoside and aglycone isoflavones three-fold greater than those by dipping method.     

高效液相色谱法测定止痛养胃软胶囊中延胡索乙素的含量

测定止痛胃软胶囊中延索乙素的含量,可用高效液相色谱法。选用甲醇—磷酸缓冲溶液(40∶60)为流动相,测定波长280nm。结果:延胡索乙素浓度在0.02140～1.37mg/mL范围内,与峰面积线性关系良好,y=(8.390×106)x+7.505×103(r=0.9997)。结论:该法操作简便、快捷、特异性强,可用于控制止痛养胃软胶囊的质量。     

微型反应器-HPLC催化合成水杨酸甲酯的研究

选择水杨酸甲酯的催化合成反应为基础反应体系，以固体超强酸为催化剂，建立微型催化反应器与高效液相色谱的联用新技术，并对液固相催化酯化反应进行微反催化合成研究。使用ZrO₂-SiO₂/SO_^2-4催化剂制成微型催化反应器进行试验，建立微反-HPLC联用实验装置，考察了水杨酸的加入量以及反应温度对转化率的影响。并通过X-射线衍射、红外光谱和电子透镜等技术，对反应前后催化剂的晶相、酸性特征峰以及催化剂的形态形貌进行了表征。