辣椒不同成熟期辣椒素、二氢辣椒素含量的变化

[目的]研究辣椒素、二氢辣椒素的分析方法,测定辣椒中3个不同成熟期辣椒素、二氢辣椒素含量,分析其变化规律.[方法]采用高效液相色谱进行分离,并鉴定其成分及含量.色谱条件:Shimadzu C18色谱柱(250mm×4.6mm,51μm),流动相:甲醇-重蒸水(4:1),流速:0.8mL/min,检测波长:280nm,柱温:30℃,进样量:10μL.峰面积与待测物浓度呈良好的线性关系,辣椒素标准曲线的回归方程是Y=8333309X+464.34,相关系数为0.9999.二氢辣椒素标准曲线的回归方程是Y=6386890X+2962.65,相关系数为0.9999.回收率在91.34%～95.94%之间.[结果]高效液相色谱法可以使辣椒中的辣椒素、二氢辣椒素完全分离并定性、定量分析.实验结果表明,随着辣椒成熟度的增加,辣椒素、二氢辣椒素的含量逐渐增加.[结论]本研究可以用于HPLC快速测定辣椒中辣椒素、二氢辣椒素.     

HPLC法检测辣椒不同部位中辣椒碱和二氢辣椒碱的含量

辣椒果实中的辣味成分包括辣椒碱及其衍生物(统称为辣椒碱类化合物),其中,引起辛辣味的主要化学成分辣椒碱和二氢辣椒碱约占总量的90%以上.本试验的目的是检测不同辣椒品种的不同部位中辣椒碱和二氢辣椒碱含量.因此建立了高效液相色谱方法,采用色谱条件为:C18色谱柱(4.6mm×250mm,5μm),1‰磷酸水溶液-乙腈(600:400)为流动相,流速为1.5mL/min,柱温为30℃,检测波长为281nm.该法简便,结果准确,可用于测定辣椒中辣椒碱和二氢辣椒碱的含量.利用该方法,检测了不同辣椒品种的不同部位中辣椒碱和二氢辣椒碱的含量,结果发现印度Teja中辣椒碱和二氢辣椒碱含量最高;辣椒果实不同部位辣椒碱和二氢辣椒碱含量的趋势为胎座>果肉>种子,为合理选择果实不同部位生产辣椒碱提供参考.     

辣椒中辣椒素类物质的检测方法及稳定性研究

目的:通过对GB/T 21266-2007中辣椒素和二氢辣椒素检测的色谱条件的优化,使辣椒素和二氢辣椒素的测定更加快速,并考察辣椒素与二氢辣椒素贮存过程中的稳定性。方法:高效液相色谱法,色谱条件为C18色谱柱(4.6mm×250mm,5μm),流动相为甲醇∶水(V∶V=70∶30),流速为1mL/min,检测波长为280nm,进样量10μL,柱温30℃。结果 :与GB/T 21266-2007的色谱条件相比,检测时间缩短了约12min。提取出的辣椒素与二氢辣椒素在室温条件下贮存一个月,其含量没有发生剧烈波动。结论:此色谱条件能对辣椒素和二氢辣椒素进行有效检测,且能明显缩短两者的保留时间;提取出的辣椒素与二氢辣椒素室温条件下短时间内能保持稳定。     

LC-MS/MS法测定食用油中的辣椒素和二氢辣椒素

建立了用氨基固相萃取小柱净化提取液,液相色谱串联质谱（LC-MS/MS）法测定食用油中辣椒素和二氢辣椒素含量的检测方法。结果表明,辣椒素在0～100 ng/mL范围内线性关系良好（R2 = 0.998 6）,平均回收率在70.6%～90.5%,相对标准偏差（RSD,n=3）在3.1%～8.9%,检出限为0.03 μg/kg;二氢辣椒素在0～20 ng/mL范围内线性关系良好（R2 = 0.998 8）,平均回收率在71.5%～100.7%,相对标准偏差（RSD,n=3）在6.0%～13.2%,检出限为0.006 μg/kg。该方法简便快速、准确可靠,是鉴别地沟油和测定食用油中辣椒素类物质的有效方法。     

辣椒素和二氢辣椒素在辣鸭脖卤制过程中的迁移规律研究

为了探究辣椒素和二氢辣椒素在辣鸭脖卤制过程中的迁移情况,本研究采用高效液相(HPLC)法检测卤制过程中辣椒提取液和辣鸭脖肉中的辣椒素和二氢辣椒素含量变化。结果显示,在卤制0~15 min期间,辣椒素和二氢辣椒素含量在卤水中明显减少,辣椒素从0.061 mg/mL降至0.013 mg/mL,二氢辣椒素从0.017 mg/mL降至0.004 mg/mL,而在卤鸭脖中,辣椒素和二氢辣椒素的含量显著增加,辣椒素增至0.158 mg/mL,二氢辣椒素增至0.063 mg/mL,在15 min后,卤水和卤鸭脖中的辣椒素和二氢辣椒素均呈波动变化,卤制45 min后辣椒素和二氢辣椒素从卤水至卤鸭脖的迁移率分别为92.3%、94.4%,表现了其在100℃的卤制条件下良好的热稳定性。本研究表明,可采用辣椒提取液卤制鸭脖产品,以辣椒主效成分辣椒素和二氢辣椒素的含量变化来控制卤制过程,为实现酱卤制品辣度的标准化生产提供研究基础。     

HPLC法测定云南省不同辣椒品种中辣椒碱及二氢辣椒碱的含量

利用超声提取法对云南省不同地区不同品种辣椒样品进行预处理,采用高效液相色谱法(HPLC)测定样品中辣椒碱和二氢辣椒碱的含量.具体方法为:采用色谱柱Hanbon Sci.&Tech.Lichrospher C18(250×4.6mm,5μm)分离,甲醇-3‰磷酸水溶液梯度洗脱(65％ ～90％,0～30min),检测波长280nm,辣椒碱和二氢辣椒碱的相对标准偏差都小于1％,平均回收率都在99％以上.该方法具有较好的分离效果和较高的稳定性,适用于云南省不同地区不同品种中辣椒碱和二氢辣椒碱含量的测定.测定结果显示云南省不同地区不同品种不同成熟度的辣椒中辣椒碱和二氢辣椒碱含量差异很大.     

高效液相色谱法测定辣椒制品中的辣椒素类物质

该研究采用了高效液相色谱法对辣椒制品中的辣椒素类物质进行检测,并对其提取条件和检测方法进行了研究。以乙醇∶水＝70∶30（V∶V）作为提取液,采用直接萃取法提取样品中的辣椒素和二氢辣椒素,以0.3%磷酸二氢钾溶液-乙腈（62:38,V:V）为流动相,检测波长230 nm,Macherey-Nagel Nucleosil120-5 C18色谱柱（4.6 mm×250 mm, 5 μm）分离。结果表明,辣椒素和二氢辣椒素在20～100 μg/mL质量浓度范围线性关系良好（R12 = 0.999 8,R22 = 0.999 9）,检出限为0.001 g/kg,加标回收率分别为93%～104%和86%～103%,相对标准偏差RSD＜5%。该方法操作简单、快速,具有良好的准确性和精密度,可有效排除香辛料物质的杂峰干扰,适合各类辣椒制品中辣椒素类物质的检测。     

高效液相色谱法测定豆瓣中辣椒素类物质含量

豆瓣是以蚕豆和辣椒作为主要原料生产的一种调味品,是西南地区尤其是四川地区的一种传统发酵食品。为了测定豆瓣中的辣味物质(辣椒素及二氢辣椒素),建立了高效液相色谱快速检测方法:色谱柱为C18反相色谱柱(250mm×4.6mm,5μm),流动相为甲醇和水(V/V,75∶25),流速1.0mL/min,柱温30℃,进样量20μL,检测波长280nm。辣椒素类物质的提取采用超声波辅助提取。结果表明:豆瓣样品中辣椒素含量在0.0161～0.0624g/kg之间,二氢辣椒素的含量在0.0142～0.0357g/kg之间,斯科维尔指数在519～1671SHU之间。     

实时直接质谱对辣椒及其制品中辣度的快速评价

辣椒是常见的调味品,对辣椒及其制品的辣度进行快速监控非常必要。该文首先对辣椒素和二氢辣椒素在实时直接质谱(direct analysis in real time mass spectrometry,DART-MS)的裂解机制进行了系统研究,进一步对DART离子源的气体解吸温度、栅网电极电压等试验条件进行了优化。结果表明,辣椒素和二氢辣椒素质量浓度在0. 50～50. 0μg/mL范围内与峰面积呈现良好线性关系。辣椒素和二氢辣椒素的检测限均为0. 1μg/g,定量限均为0. 5μg/g,回收率范围分别为79. 74%～97. 74%,85. 60%～98. 71%,精密度分别为0. 80%～8. 89%,2. 69%～9. 54%。该方法可用于辣椒及其制品中辣度的快速评价。     

不同产地辣椒中辣椒素含量测定研究

建立高效液相色谱法测定不同产地辣椒中辣椒素的含量。采用ShimadzuC18色谱柱(4.6×150mm,5μm),流动相:乙腈-0.4%磷酸(41∶59),流速:1.0mL/min,检测波长:280nm,柱温:室温,用外标法定量。结果表明,辣椒素的线性范围3.70~14.80μg,r=0.9991,回收率100.16%,RSD2.49%。该方法简便,快速,线性关系良好,适合辣椒中辣椒素的含量测定。     

Capsaicinoids,Tocopherol, and Sterols Content in Chili (Capsicum sp.) by Gas Chromatographic-Mass Spectrometric Determination

A gas chromatography-mass spectrometry method was developed for the quantitative determination of capsaicinoids, vitamin E, and phytosterols in chili peppers using a simple extraction technique for rapid screening. These components were extracted with acetonitrile and were injected into gas chromatography attached with mass spectrometry. The mean recovery values for triplicate analysis were between 90.6–99.7%. Besides major capsaicinoids (capsaicin, dihydrocapsaicin, nordihydrocapsaicin), four more minor capsaicinoids (nonivamide, nornordihydrocapsaicin, homodihydrocapsaicin I and II) were detected in chili samples. α-Tocopherol was also detected in the same run along with three phytosterols (campesterol, γ-sitosterol, and stigmasterol). Variations were observed across the chili sample in all of the constituents except a few minor capsaicinoids. The method was suitable for simultaneous estimation of capsaicinoids, vitamin E, and phytosterols in a single run from any types of pepper. Thus, the method is effective for rapid screening of peppers for its nutraceutical composition using single solvent extraction.     

Studying the Effect of Household-Type Treatment and Processing on the Residues of Ethion and Profenofos Pesticides and on the Contents of Capsaicinoids in Green Chili Pepper Using GC-MS/MS and HPLC

The first aim of this study was to create, test, and apply a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, based on acetonitrile extraction, for simultaneous determination of pesticide residues in green chili pepper (fresh and dried forms). There is a group of 86 repeatedly detected pesticides in the agricultural food commodity in Al-Qassim region, Saudi Arabia. The suggested method is utilizing GC-MS/MS for simultaneous determination of those 86 pesticides. The limit of quantitation (LOQ) for each pesticide was set as the lowest fortification level that achieved acceptable recoveries in the range 70–120% with precision (RSD ≤ 20%). The results indicated that two organophosphorus pesticides, ethion and profenofos, in the analyzed chili pepper samples have significantly exceeded the European maximum residual limit (MRL) for pesticides. The second purpose of the study was to evaluate the effect of some different household-type treatment and processing procedures on the detected pesticide residues and on capsaicinoids (particularly, capsaicin and dihydrocapsaicin) which are responsible for the pungency of chili pepper, using GC-MS/MS and HPLC. Some recommendations were concluded for the best practices.     

HPLC Analysis of Capsaicinoids Extracted from Whole Orange Habañero Chili Peppers

ABSTRACT: A rapid, single-stage, quantitative extraction procedure is described for high-performance liquid chromatographic (HPLC) analysis of capsaicin and dihydrocapsaicin in whole chili peppers. Individual and multiple Capsicum chinense (orange habañero) pepper samples were analyzed in a 2 y study. Peppers, both undried and dried, contained average values of 1250 ppm capsaicin and 540 ppm dihydrocapsaicin relative to undried weight. Relative to dry weight, the orange habañero peppers contained 8840 ppm capsaicin and 3940 ppm dihydrocapsaicin.     

云南省主要辣椒品种活性成分及其加工适应性

目的 研究云南不同品种辣椒活性成分的差异,并讨论其加工适应性。方法 以49份云南辣椒材料为研究对象,测定不同辣椒材料中总黄酮、总酚、总生物碱、总皂苷、维生素C、降二氢辣椒碱、辣椒碱和二氢辣椒碱的含量,利用相关性分析、主成分分析法与聚类分析法进行综合评价。结果 主成分分析将8项活性成分指标综合为3个主成分,其累计方差贡献率为71.774%。经综合评价,得分前3位的辣椒品种分别是49号(小米辣,小米辣)、35号(川优19,干椒)、43号(晶翠,小米辣),具有较高的综合加工适应性。采用聚类分析方法可将49份云南辣椒材料分为3类。其中35号(川优, 19干椒)、43号(晶翠,小米辣)、48号(朝天椒,朝天椒)聚为一类,可用于提取辣椒碱、辣椒油树脂等产品。49号(小米辣,小米辣)为云南本土调味品企业泡制加工用小米辣,被单独聚为一类,综合得分最高,综合加工适应性最佳。结论 采用主成分与聚类分析作为评价辣椒加工适用性的统计学分析手段,能够有效区分不同辣椒品种的活性特征,对进一步开发云南地区的辣椒资源、评价其加工适用性有一定的指导意义。     

Fast Separation of Capsaicinoids from Peppers by Reversed Phase Ultra-Performance Liquid Chromatography: Comparation with Traditional High-Performance Liquid Chromatography Methods

A new chromatographic method for the separation of major capsaicinoids in peppers has been developed. Nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin have been separated by reversed-phase ultra-performance liquid chromatography. A gradient method has been developed using two solvents: 0.1% acetic acid in water and 0.1% acetic acid in methanol. The developed method allows the full separation of capsaicinoids in less than 3 min, with high reproducibility (relative standard deviation < 4.3%) and repeatability (relative standard deviation < 3.6%). Robustness regarding the total amount of methanol in the sample was determined. Comparison with previous reversed-phase high-performance liquid chromatography methods using both monolithic and conventional columns was also studied. Finally, the method was applied in the determination of major capsaicinoids in 16 hot pepper samples produced in Spain.     

Capsaicinoid Contents in Peppers and Pepper-Related Spicy Foods

The quantification of the major capsaicinoids, namely nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin, present in spicy foods made from peppers has been performed. The capsaicin content is directly related to the pungency properties of foods that contain hot peppers. The samples studied included 10 different dried hot peppers, 19 hot sauces, 4 kinds of paprika, and 4 different ketchups. The range of concentrations of capsaicinoids found were as follows: dried hot peppers (554.1–1705.9 mol kg^?1), paprikas (582.0–665.0 mol kg^?1), spicy ketchups (4.0–12.4 mol kg^?1), and hot sauces (4.6–843.8 mol kg^?1). Variability in the capsaicinoid content was found, with capsaicin and dihydrocapsaicin present at the highest levels. The capsaicin content was generally higher than the dihydrocapsaicin content.     

Fast determination of capsaicinoids from peppers by high-performance liquid chromatography using a reversed phase monolithic column

This article reports the development of a rapid and reproducible method of HPLC with fluorescence detection for the determination and quantification of the main capsaicinoids (nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin and homodihydro-capsaicin) present in hot peppers by employing a monolithic column. The type of column employed is a RP-18e (100 mm × 4.6 mm) monolithic column. A gradient method was utilised for the chromatographic separation: solvent A: water (0.1% acetic acid) and solvent B: methanol (0.1% acetic acid). A study was also made of the robustness of the method in respect of the conditions of temperature in the separation column (15–40 °C), the solvent flowrate (4–7 mL min⁻¹), the injection volume (10–50 μL), and the percentage of methanol in the sample (25–100%). The repeatability and reproducibility of the method showed relative standard deviations of less than 2%. The robustness of the method was determined by utilising different injection volumes and different percentages of methanol in the extracts. The method developed has then been utilised for the quantification of the major capsaicinoids present in different varieties of hot peppers grown in Spain. The capsaicinoids have been separated in a time of less than 8 min.     

Determination of capsaicinoids in foods using ultra high performance liquid chromatography

A sensitive, precise, and specific ultra high performance liquid chromatographic (u-HPLC) method was developed for the analysis of capsaicin in foods. The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The u-HPLC separation was performed on a reversed column C₁₈ (particle size 2 μm, i.d. 2 mm, length 50 mm, followed by fluorescence detection-excitation 280 nm, emission 325 nm). The recovery of capsaicin in gochujang was more than 91%, and the detection limit and lower determination limit of u-HPLC analysis were 0.054 and 0.163 μg/mL for capsaicin and 0.053 and 0.160 μg/mL for dihydrocapsaicin, respectively. The calibration graph for capsaicin and dihydrocapsaicin was linear from 0.2 to 10.0 μg/mL for u-HPLC analysis. The inter-day and intra-day precisions (relative standard deviations) were <5.21% for capsaicin and <9.79% for dihydrocapsaicin while the average recoveries obtained were quantitative 91.1–94.8% for capsaicin, 91.4–97.0% for dihydrocapsacin, indicating good accuracy of the u-HPLC method.