高效液相色谱法(HPL)测定藏花素的研究

采用高效液相色谱法（HPLC）,选用TunerPackingKromasil氨基柱,以乙腈：水（80：20）为流动相,流速08ml／min,440nm下测定藏花素,结果表明：藏花素的保留时间为1219min,最小检测限为12．5ng,加样回收率为99．34％,色谱峰分离效果好,具有良好的稳定性和重视性。     

高效液相色谱法（HPLC）测定栀子中栀子甙的含量

采用高效液相色谱法,选用ＹＷＧ－Ｃ８反相柱,以甲醇－水－磷酸分离测定栀子中的栀子甙。栀子甙具有良好的线性关系和分离度、稳定性和重现性好,平均回收率为９９．０１％、本文对栀子全果,皮,种子进行测定,其栀子甙含量分别为３．１５０ｇ／１００ｇ,２．２９４ｇ／１００ｇ,３．３１５ｇ／１００ｇ。     

高效液相色谱法测定糕点中的栀子黄

目的改进GB/T5009.149-2003《食品中栀子黄的测定第一法高效液相色谱法》的方法。方法样品经甲醇:甲酸(6:4,V:V)洗脱,采用Angilent Extend C_(18)反相色谱柱(4.6 mm×250 mm,5μm),以甲醇:0.2%氨水(50:50,V:V)为流动相(等度洗脱),流速为1.0 mL/min,进样量20μL,经配有二极管阵列检测器(DAD)的高效液相色谱仪(high performance liquid chromatograph,HPLC)进行测定。结果本方法检出限为3.2 mg/kg,栀子黄中藏花酸和藏花素峰面积的相对标准偏差分别为1.6%、2.5%,在5~50μg/mL范围内有较好的线性,Y=1.34X-0.54,r~2=0.9998,不同浓度的回收率在91.2%~98.4%之间。结论本方法简单、高效、准确度高,回收率和重现性良好,适用检测的食品类别范围较宽,具有推广应用价值。     

高效液相色谱法测定食品中的栀子黄的研究

对国家标准（GB/T5009．149—2003）中的高效液相色谱测定食品中栀子黄进行了研究，通过不同溶液中栀了黄色素含量的分析，用吸光度法作对照。结果表明：国标中以栀子苷为对照品，用高效液相色谱法测定食品中的栀子黄色素不够合理。为建立成熟的定性、定量栀子黄色素的方法奠定了基础。     

高效液相色谱法测定栀子中藏花素的含量

建立了一种用高效液相色谱法测定栀子中藏花素含量的方法。采用XBridge Amide氨基柱(150mm×4.6mm,5μm),以甲醇∶乙腈∶水(17∶33∶50)为流动相,流速1.0ml/min,检测波长440nm,柱温25℃,用外标法定量,测定栀子中藏花素的含量。结果表明,测定藏花素的线性回归方程为y=1.508 7x-0.014 1,相关系数R2=0.996 2,回收率97.68%,相对误差0.729%,该方法简便,快速,线性关系良好。     

高效液相色谱法测定肉制品中栀子黄色素含量

通过正交试验分析法对肉制品中栀子黄色素提取方法进行优化。利用正交试验设计考察提取溶剂体积、超声时间和提取次数对肉制品中栀子黄色素提取回收率的影响。结果表明,肉制品中栀子黄色素的最优提取条件为：甲醇为提取溶剂、固液比1∶6（g/mL）、超声提取时间20 min、提取2 次;建立高效液相色谱法测定肉制品中栀子黄色素中藏花素和藏花酸方法的线性范围为0.5～50 mg/mL,相关系数大于0.999,检出限不高于0.07 μg/g,加标平均回收率为83.51%～96.00%,相对标准偏差不大于2.94%。该方法准确度高、简单、快速,可适用于肉制品中栀子黄色素中藏花素和藏花酸含量检测。     

高效液相色谱法测定奶粉中的β—胡萝卜素

采用高效液相色谱法测定奶粉中的β－胡萝卜素。奶粉样品在甲醇溶剂中碱化后,用石油醚萃取β－胡萝卜素,经Ｖａｒｉａｎ３０ｃｍ×４ｍｍ硅胶柱分离,紫外检测定量,该方法最低检出限为５．３８×１０－１０ｇ,回收率为９５．３％～９８．４％,变异系数ＣＶ（％）为２．０４％     

多杀菌素的高效液相色谱测定

本文建立了高效液相色谱法测定多杀菌素的定量分析方法,本方法的相对标准偏差为1.3441,变异系数为1.8067%,线性相关系数为0.99959,平均回收率达到99.2429%,最后采用液质联用方法对目标化合物进行验证.     

Determination of Chlorantraniliprole Residues in Grape by High-Performance Liquid Chromatography

An effective analytical method for the residue analysis of a novel insecticide chlorantraniliprole and its dissipation in grape were studied. Chlorantraniliprole residues were extracted from grape samples with ethyl acetate. The extract was cleaned up with QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and determined by high-performance liquid chromatography with photodiode array detector (HPLC-DAD). At fortification levels of 0.06, 0.5, and 1.0 mg kg^?1 in grape, it was shown that recoveries ranged from 95.11 to 102 % with relative standard deviation (RSD) of 6 to 11 %. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.02 and 0.06 mg kg^?1, respectively. The dissipation half-life time of chlorantraniliprole residues in grape was 2.70 days. According to maximum residue limit (MRL), the preharvest interval (PHI) of chlorantraniliprole on grape was 4 days after the treatment. Based on the results of this study and the relevant residue regulation, chlorantraniliprole residue levels will be acceptable when applied to grape in Egypt.     

高压液相色谱法测定大豆异黄酮含量

大豆试样在酸性条件下水解后,采用岛津LC-10AtvpHPLC仪,紫外检测器(SPD-10Avvp),波长 254 nm,色谱柱:Inertsil ODS-3柱(5μm,4.6 mm×250 mm),流动相:甲醇:5％ 醋酸溶液30％～70％梯度洗脱,流速:1.0 ml/min,柱温:50℃条件下,测定水解提取物中大豆异黄酮含量。测定结果表明:不同品种、产地的大豆中异黄酮含量为 1.40 mg～3.30 mg/g,大豆胚芽中异黄酮含量最高,为13.18mg/g;其它豆类,如红豆、绿豆、青豆、豌豆等异黄酮含量为0.37mg～1.2mg/g,此测定法能为大豆的选育种、栽培及大豆异黄酮含量评价提供依据。     

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.     

Simultaneous Determination of Thiamin and Riboflavin in Selected Foods by High-Performance Liquid Chromatography

A high-performance liquid chromatographic (HPLC) system that makes it possible to accurately and simultaneously quantitate low levels of riboflavin and thiamin (thiochrome) from single extracts following oxidation and sample preconcentration steps is described. Several food matrices were analyzed and the results compared to the AOAC method now in use. Within the range of standard deviations, both methods gave comparable values. This method is rapid, accurate, sensitive and economical, making it attractive to those who require routine analysis of thiamin and riboflavin.     

高效液相色谱法同时测定香肠中6种生物胺

采用丹磺酰氯为衍生试剂,建立反相高效液相色谱法同时测定香肠中腐胺、尸胺、酪胺、组胺、亚精胺和精胺6种生物胺的方法.色谱条件:C18色谱柱分离,以甲醇和0.1%乙酸溶液为流动相梯度洗脱,流速0.8mL/min,二极管阵列检测器,检测波长254 nm.以1,7-二氨基庚烷为内标,在设定的试验条件下,6种生物胺实现了良好的分离,并呈良好的线性相关性(r>0.999).方法的检测限:腐胺、亚精胺、尸胺和酪胺均为0.8μg/mL,组胺和精胺均为4 μg/mL.本检测方法具有良好的重现性和回收率.对发酵香肠样品中的生物胺含量进行了分析,其中部分香肠中含有一定量的生物胺,最高可达1.09mg/g.     

Quantitative Determination of Isoflavones in Soy Based Nutritional Supplements by High-Performance Liquid Chromatography

An increasing number of nutritional supplements contain phytoestrogens, in particular isoflavones, which potentially alleviate climacteric complaints. Intention of the present study was the qualitative and quantitative determination of isoflavones in soy based nutritional supplements in order to compare the actual content with the labeling of these products. For the analysis high-performance liquid chromatography (HPLC) with photo diode array (PDA) detection was used. The amount of isoflavones was determined via external calibration functions. Our analyses revealed certain variations in the isoflavone content of soy based nutritional supplements, with regard to the individual and the total amount. Furthermore, the total amount of isoflavones per serving unit in some products was higher than declared on the labeling, although only the major isoflavones were taken into account. This study shows that there is the necessity to clearly specify the isoflavone composition on the labeling and - due to safety aspects - to standardize and control the isoflavone content.

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Zusammenfassung:  Nahrungserg?nzungsmittel mit Zusatz von Soja werden vermehrt als “Alternative” zur klassischen Hormonersatztherapie für Frauen im Klimakterium angeboten. Diese Pr?parate enthalten Isoflavone, welche zu den Phytoestrogenen z?hlen und eine estrogene Wirkung aufweisen. Die in Sojabohnen enthaltenen Isoflavone sollen unter anderem klimakterische Beschwerden wie z.B. Hitzewallungen oder Tachykardie lindern. In der vorliegenden Studie wird eine Methode beschrieben, mit der aus Nahrungserg?nzungsmitteln mit Zusatz von Soja-Extrakten der Gehalt an Isoflavonen bestimmt werden kann. Dazu wurde eine HPLC-Methode mitDioden-Array-Detektion entwickelt, mit welcher die Quantifizierung der in Soja vorliegenden Isoflavone über externe Kalibrierfunktionen erfolgen kann. Damit war es m?glich, die vom Hersteller gemachten Angaben bezüglich der Isoflavongehalte zu überprüfen. Unsere Untersuchungen wiesen deutliche Unterschiede sowohl im Gesamtgehalt an Isoflavonen als auch in der individuellen Zusammensetzung der einzelnen Produkte auf. In einigen F?llen war der Isoflavongehalt in einigen Produkten pro Verzehrseinheit deutlich h?her als vom Hersteller angegeben. Unsere Untersuchungen belegen die Notwendigkeit im Sinne des Verbraucherschutzes, die Isoflavongehalte in Nahrungserg?nzungsmitteln klar zu spezifizieren und zu deklarieren.

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Received: January 9. 2008; accepted: February 19. 2008     

高效液相色谱法测定食品中番泻苷A和番泻苷B的含量

建立高效液相色谱法测定食品中番泻苷A和番泻苷B的方法。样品经过0.2%碳酸氢钠溶液超声提取,采用Agilent ZORBAX SB-C₈(4.6 mm×150 mm,5.0 μm)色谱柱分离,以四氢呋喃-水-乙酸为流动相洗脱,DAD检测器,检测波长:340 nm。番泻苷A、番泻苷B在1～100 μg/mL范围线性关系良好,相关系数均大于0.999,检出限(S/N=3)为15 mg/kg,定量限(S/N≥10)为50 mg/kg。以空白样品进行添加回收试验,番泻苷A的回收率为80.88%～96.34%,相对标准偏差(Relative Standard Deviation)为3.07%～7.73%,番泻苷B的回收率为81.32%～102.2%,相对标准偏差(RSD)为2.62%～9.62%。该方法前处理简单、灵敏度高、操作简便、准确性良好。在市售的果冻类食品中,检出阳性样品。