免疫亲和柱-高效液相色谱法检测红曲米中的桔霉素

制备抗桔霉素(citrinin,CIT)单克隆抗体免疫亲和柱(IAC),建立了检测红曲米中CIT的免疫亲和柱-高效液相色谱检测方法。采用甲醇-水提取红曲米样品,将提取液用PBS稀释后过免疫亲和柱,甲醇洗脱后以高效液相色谱法检测,激发波长为331 nm,发射波长为500nm,流动相采用乙腈-磷酸溶液(体积比为45:55,pH2.0)。每根抗CIT单克隆抗体免疫亲和柱使用0.5 mL溴化氰活化的4FF琼脂糖凝胶,0.5mg桔霉素单克隆抗体,柱容量为0.35μg。红曲米样品添加CIT标品0.1～0.6 mg/kg,平均回收率为74.2%～87.14%,相对标准偏差为2.85%～13.12%。最低检出限为0.1mg/kg(S/N=3)。     

超高效液相色谱-串联质谱法测定红曲类保健品中的桔青霉素

建立了高效液相色谱-串联质谱对红曲类保健品中的桔青霉素含量进行检测的方法.采用70％甲醇-水溶液提取样品,经HLB固相萃取小柱净化后,通过高效液相色谱-串联质谱法测定桔青霉素的含量,多反应监测(MRM)方式监测离子对m/z251→233(桔青霉素)外标法定量.结果表明,桔青霉素基质曲线在浓度5～100 ng/mL范围内...     

基于红曲高产莫纳可林K的固态发酵工艺条件优化

利用响应面法优化红曲固态发酵产莫纳可林K的工艺条件。在采用变温发酵,发酵时间固定的条件下,单因素试验研究接种量、装料量、玉米粉添加量和蛋白胨添加量等4个因素对红曲固态发酵莫纳可林K产量的影响。在此基础上,应用Design-Expert软件建立数学模型,进行四因素三水平的响应面分析。结果表明,红曲固态发酵高产莫纳可林K工艺条件为接种量17.50%,装料量32.95 g/250 mL、玉米粉添加量3.80%和蛋白胨添加量2.37%。此条件下进行验证试验,莫纳可林K产量为11.25 mg/g,与回归方程预测值无显著差异,说明该法优化红曲固态发酵过程中莫纳可林K的产量可行。     

正交试验设计优化茶藨子木层孔菌总多糖的提取条件

目的研究提取茶藨子木层孔菌总多糖的最佳条件。方法用蒽酮-硫酸法测定总多糖含量,以提取温度、时间、次数、溶剂用量等4项因素,设计3个水平进行正交试验。结果最佳工艺为15倍量水,90℃提取4h,共3次。结论本实验确定的最佳条件稳定性好且简便易行。     

正交试验设计优化茶藨子木层孔菌总多糖的提取条件

目的 研究提取茶藨子木层孔菌总多糖的最佳条件.方法 用蒽酮-硫酸法测定总多糖含量,以提取温度、时间、次数、溶剂用量等4项因素,设计3个水平进行正交试验.结果 最佳工艺为15倍量水,90℃提取4 h,共3次.结论 本实验确定的最佳条件稳定性好且简便易行.     

酸法苇浆红液提取工程的改造及工艺条件优化

本文详细介绍了亚硫酸盐苇浆红液进口提取系统的工艺流程、工艺参数及操作特点，并针对此系统在改造生产实践中出现的诸多问题进行解决及改进，实现了自动化生产和绿色生产的双重目标。     

红曲的生产工艺及Monacolin K和桔霉素的检测

综述红曲的生产工艺及Monacolin K和桔霉素的检测方法,指出采用新型生产工艺、优化发酵条件和应用菌种筛选等现代技术是生产既富含活性成分Monacolin K又不合桔霉素的功能性红曲的重要途径,同时预示Monacolin K和桔霉素检测技术的进展将为功能性红曲产品的质量、安全使用及国际市场的开拓提供技术支撑.     

红曲米中桔霉素、淀粉、水分含量的快速测定

采用近红外光谱技术构建红曲米中桔霉素、淀粉、水分含量的快速测定预测模型。分别采用偏最小二乘回归(PLS)、主成分回归(PCR)、多元线性回归(SMLR)构建所测组分的数学模型,以相关系数(R)、预测相对分析偏差(RPD)、预测均方根误差(RMSEP)、校正均方根误差(RMSEC)值来评价模型的综合性能。结果表明,MSC、SNV方法可以消除样品颗粒不均对光谱的散射影响;导数处理能够消除基线漂移问题;对于水分含量,只有PLS和PCR模型可用于较准确定量测定(RPD=2.45和2.81);对于淀粉,只有SMLR模型可用于较准确定量测定(RPD=2.58);对于桔霉素,3种模型的RPD值均小于2,虽然不能用于准确定量测定,但能满足定性分析或分级。为红曲米生产过程中桔霉素、淀粉、水分含量的快速检测提供新的方法,为红曲米质量的智能化控制提供新的途径。     

Citrinin Determination in Red Fermented Rice Products by Optimized Extraction Method Coupled to Liquid Chromatography Tandem Mass Spectrometry (LC‐MS/MS)

A rapid and sensitive method was developed and validated for citrinin determination in red fermented rice products by liquid chromatography tandem mass spectrometry (LC‐MS/MS) under the selected reaction monitoring mode. Sample preparation was especially focused, and the quantitative methods of LC‐MS/MS and high‐performance liquid chromatography with fluorescence detection (HPLC‐FLD) were compared. In red fermented rice samples, the limit of detection was 1.0 μg/kg for LC‐MS/MS compared to 250 μg/kg for HPLC‐FLD, the limit of quantification was 3.0 μg/kg for LC‐MS/MS compared to 825 μg/kg for HPLC‐FLD. High correlation coefficient was obtained (R² = 0.999) within the linear range (0.1 to 100 μg/L) in the MS method. The recoveries ranging from 80.9% to 106.5% were obtained in different spiking concentrations. The average intra‐ and inter‐day accuracy ranged from 75.4% to 103.1%, and the intra‐ and inter‐day precisions were from 3.3% to 7.9%. The developed method was applied to 12 commercial red fermented rice products, and citrinin was found in 10 samples ranging from 0.14 to 44.24 mg/kg. Compared to traditional qualitative and quantitative methods, the newly developed LC‐MS/MS method for citrinin determination includes the merits of using a small amount of extraction solvent, simple preparation steps, and high sensitivity.     

超声波辅助提取红树莓籽油工艺优化

研究红树莓籽油的超声波辅助浸提工艺。以出油率为指标,在单因素试验的基础上,通过正交试验确定超声波辅助提取红树莓籽油的最佳工艺条件。结果表明,在超声波功率100W、提取温度30℃、提取时间25min、料液比1:11(g/mL)的条件下,红树莓籽的出油率最高为12.97%。     

Determination of 13 Phenolic Compounds in Rice Wine by High-Performance Liquid Chromatography

Rice wines are widely consumed by the general public in Asian countries, while comprehensive studies focused on the individual phenolic compounds in rice wines are limited. A rapid method for simultaneous determination of 13 phenolic compounds in rice wines by high-performance liquid chromatography (HPLC) was developed and validated, and the phenolic compounds in commercial rice wine samples (Chinese rice wine, Japanese sake, and Korean makgeolli) were determined in this paper. The identified compounds contained gallic acid (GA), protocatechuic acid (PRCA), vanillic acid (VA), syringic acid (SRA), caffeic acid (CA), ferulic acid (FA), p-coumaric acid (pCA), sinapic acid (SA), chlorogenic acid (CHA), (+)-catechin (CAT), (?)-epicatechin (EPI), quercetin (QUE), and rutin (RUT). Phenolics were separated with a C18 reversed-phase column at 38 °C by gradient elution using 3 % acetic acid aqueous solution (solvent A) and acetonitrile (solvent B) (0 min, 5 % B; 5 min, 8 % B; 10 min, 15 % B; 20 min, 25 % B; and 25 min, 5 % B) as the mobile phase at 280 nm with flow rate of 1.0 mL min^?1. With direct injection of rice wine samples, the chromatograms of all analytes were observed within 20 min, all calibration curves were linear (R ²?>?0.995) within the range, limits of detection (LOD) ranged from 0.02 to 0.06 μg mL^?1, and good recoveries (88.07–106.80 %) and precision (relative standard deviation (RSD)?<?5.36 % ) were obtained for all compounds. This method was applied to quantify phenolic compounds in commercial rice wine samples (Chinese rice wine, Japanese sake, and Korean makgeolli), and good separation peaks were observed and catechin was the predominant phenolic in the samples. The average values of total phenolic contents of the three groups of rice wine were significantly different (p?<?0.01). In conclusion, this procedure can be used to determine the phenolic compounds in various types of rice wines, as well as to characterize and differentiate rice wine samples.     

pH精制区带逆流色谱分离制备红曲中的酸式莫那可林K

建立了pH精制区带逆流色谱分离制备红曲中功能成分酸式莫那可林K的新方法。首先用体积分数95%乙醇提取红曲中的莫纳可林K,然后经过碱化处理使内酯式莫那可林K转化为酸式,最后采用溶剂系统V(石油醚):V(乙酸乙酯):V(甲醇):V(水)=5:5:4:6,上相添加HCl(10mmol/L)作为固定相,下相添加氨水(10mmol/L)为流动相进行pH精制区带逆流色谱分离。分离所得的酸式莫那可林K经HPLC检测纯度,并用UV,ESI-MS和~1H-NMR鉴定其化学结构。从2.0g粗提物一次分离得到纯度为93.4%的酸式莫那可林K147mg。     

用双向薄层层析检测红曲中的桔霉素

采用双向展开薄层层析检测红曲中的桔霉素，第一相分离红曲中除桔霉素外的其他成分，第二相主要分离桔霉素。第一相展开剂选择氯仿：丙酮＝9：1，第二相展开剂选用苯：乙酸乙酯：甲酸＝6：3：1。结果表明，最小检出量为0.1μg，可检测出红曲中的桔霉素，方法简单易行，容易掌握。（庞晓）     

正交试验法优化米饭汉堡制备工艺条件

研制一种新型中式米制快餐食品——米饭汉堡,并对其工艺条件进行优化。通过单因素试验考察不同粳米糯米比、米水比、浸泡时间和品质改良剂对米饭汉堡质构特性的影响。以感官评价为依据,通过正交试验得到米饭汉堡的优化工艺条件为粳米糯米比3:7、米水比1:1、SSPS添加量0.2%。通过上述优化工艺条件制得的米饭汉堡品质最佳。     

正交设计优选苦荞中芦丁和槲皮素的提取工艺研究

试验优选了乙醇回流提取苦养中芦丁和槲皮素的最佳工艺条件.采用单因素和正交设计法考察乙醇浓度、料液比、提取时间3个因素对苦荞中黄酮类化合物提取率的影响,利用高效液相色谱仪测定苦荞中芦丁和槲皮素的含量,以其含量为指标优选工艺.结果表明最佳工艺为:以70%乙醇为溶剂,1:20料液比,提取时间2 h.该提取工艺合理、可行,可为...     

正交试验优化马铃薯龙葵素提取技术

以变绿、发芽的马铃薯皮为原料,在系统优化筛选双溶剂提取法、超声波辅助提取法提取马铃薯龙葵素的基础上,比较乙醇回流提取、微波辅助提取、双溶剂提取、超声波辅助提取4种方法对马铃薯龙葵素的提取效果。结果表明,双溶剂提取马铃薯龙葵素的最佳工艺为提取温度70℃、提取时间17h、料液比1:20、乙醇乙酸比10:2、原料粒径0.3mm,龙葵素得率为0.6417%,4个因素对马铃薯龙葵素提取效果的影响大小为乙醇乙酸比>粒径>料液比>时间;超声波辅助提取的最佳工艺为70%乙醇、pH3、超声温度65℃、超声时间为20min、料液比为1:15、原料粒径0.3mm、超声2次,龙葵素得率达到0.8356%,4个因素对马铃薯龙葵素提取效果的影响大小为粒径>料液比>超声温度>超声时间;微波辅助提取和乙醇回流的提取得率分别为0.5489%、0.1881%。比较4种提取方法,超声波辅助提取时间短,溶剂用量少,提取效果最好。     

Analyses of Glycolipids in Clove, Red Pepper, and Nutmeg by High-Performance Liquid Chromatography

ABSTRACT: To determine the existence of glycolipids (neutral glycosphingolipid and glycoglycerolipid) in clove, red pepper, and nutmeg, we performed silica gel chromatography and high-performance liquid chromatography (HPLC) using an Aquasil-SS column and a C₈-reversed-phase silica gel column. HPLC (Aquasil-SS column) with a UV absorption detector was used to analyze neutral glycosphingolipid. These chromatograms showed two typical peaks in clove lipids. UV-HPLC (C₈-reversed phase silica gel column) was also used to analyze glycoglycerolipid. The chromatograms indicated a small peak in clove lipids. Moreover, we observed the same two peaks in the glycolipid fraction of clove lipid when we used HPLC (Aquasil-SS column) with a differential refractometer detector. These results suggest that clove may contain new and plural neutral glycosphingolipids.     

Optimization of Rice Bran Fermentation Conditions Enhanced by Baker’s Yeast for Extraction of Protein Concentrate

The rice bran fermentation conditions for extraction of protein concentrate was enhanced by the use of baker’s yeast at optimized conditions using response surface methodology (RSM). A central composite design with three independent variables: fermentation temperature (25 to 35°C), yeast concentration (1 to 5%) and fermentation time (10 to 24 h) was used to study the response variable (protein yield). Results indicated that the generated regression model represented the relationship between the independent variables and the responses. Also, all linear terms, two quadratic terms (fermentation temperature and time) and all interactive terms had significant (p < 0.05) effect on the protein yield. The optimum conditions for yeast pretreatment of rice bran protein extraction were achieved at 30°C for 17 h using 3% yeast concentration to obtain a protein yield of 23.37%, which showed no significant difference (p > 0.05) from the response surface methodology predicted protein yield (23.02%). The use of baker’s yeast in the fermentation of rice bran for extraction of protein concentrate can be more effectively used to improve the extraction yield compared to natural fermented (15.43%) and untreated rice bran (10.16%).     

Determination of Anthraquinone Derivatives in Chang-Qing Tea by Using Cloud-Point Extraction and High-Performance Liquid Chromatography

In this paper, a cloud-point extraction method was developed for the determination of five anthraquinone derivatives in Chang-Qing tea by high-performance liquid chromatography. The optimum conditions for micelle extraction were obtained as follows—15% (w/v) Genapol X-080 as extractant, pH 3.5, liquid/solid ratio 80, and extraction time, 40 min. For cloud point preconcentration, 20% (w/v) NaCl was added, and the solution was incubated at 55 °C for 30 min. The detection limits for the five anthraquinone derivatives were in the range of 0.55–3.30 ng ml⁻¹. Average recoveries for the anthraquinone derivatives at three spiked levels were in the range of 84.3–104.1%. Relative standard deviations for six replicate determinations of Chang-Qing tea sample were below 2.39. The established method has been successfully applied to the determination of anthraquinone derivatives in Chang-Qing tea products from three different manufacturers.     

正交旋转设计优化萝卜籽硫甙提取工艺

本研究在单因素试验的基础上,选定浸提温度、水料比、提取时间三个因素进行正交旋转组合试验,对萝卜籽中硫甙提取工艺进行了研究,建立了硫甙得率的二次回归方程。此模型拟合性好,通过响应面分析以及模拟寻优得到了优化组合条件。结果表明,温度对硫甙得率有显著的影响,水料比和浸提时间对硫甙得率有影响但不显著。当提取温度4.3～16.5℃,浸提时间20～57min,水料比9.4～14.2ml/g时,硫甙提取液浓度可达到0.9mg/ml以上。