余永昊,谢定源,方妍,范刚,丁璐

• 1:华中农业大学食品科学技术学院环境食品学教育部重点实验室

摘要(Abstract)：

利用固相萃取技术对辣椒油中辣椒素类物质的提取分离工艺进行优化,并采用高效液相色谱对优化后的工艺进行辣椒素类物质回收率的检验。辣椒油制备的最佳料液比为1∶4(g/g),通过对稀释剂体积、洗脱剂种类和洗脱剂体积3个因素进行单因素实验和正交实验,结果表明固相萃取提取分离辣椒油中辣椒素类物质的最佳条件为:稀释剂用量为2mL,洗脱剂为90%甲醇-乙腈溶液,洗脱剂体积为4mL,此时辣椒素类物质的提取量最多。用标品检验最佳条件下辣椒素类物质的回收率,为84.3%～98.6%,说明固相萃取提取辣椒油中辣椒素类物质的提取率高。日间精密度和日内精密度相对标准偏差为0.2%～3.2%,说明优化工艺精密度高、稳定性好。利用优化方法后的固相萃取法提取分离辣椒油中的辣椒素类物质,可以去除样品中的油脂,减少样品对色谱柱的污染,大大延长色谱柱的使用寿命。

关键词(KeyWords)： 辣椒油;辣椒素;固相萃取(SPE);高效液相色谱(HPLC)

Abstract:

Keywords:

基金项目(Foundation): 十三五国家重点研发计划项目(2017YFD0400101)

作者(Author): 余永昊,谢定源,方妍,范刚,丁璐

参考文献(References)：

• [1]García-Gaytán V,Gómez-Merino F C,Trejo-Téllez L I,et al.The chilhuacle chili(Capsicum annuum L.)in Mexico:description of the variety,its cultivation,and uses[J].International Journal of Agronomy,2017(5):1-13．
• [2]ChamikaraM D M,Dissanayake D,Ishan M,et al.Dietary,anticancer and medicinal properties of the phytochemicals in chili pepper (Capsicum spp.)[J].Ceylon Journal of Science,2016,45(3):5-20．
• [3]Srinivasan K.Biological activities of red pepper (Capsicum annuum)and its pungent principle capsaicin:a review[J].Critical Reviews in Food Science and Nutrition,2016,56(9):1488-1500．
• [4]Chapa-Oliver A M,Mejía-Teniente L.Capsaicin:from plants to a cancer-suppressing,2016,21(8):931．
• [5]Varghese S,Kubatka P,Rodrigo L,et al.Chili pepper as a body weight-loss food[J].InternationalJournalofFoodSciences and Nutrition,2017,68(4):392-401．
• [6]Lavorgna M,Orlo E,Nugnes R,et al.Capsaicin in hot chili peppers:in vitro evaluation of its antiradical,antiproliferative and apoptotic activities[J].Plant Foods for Human Nutrition,2019,74(2):164-170．
• [7]Zheng J,Zheng S,Feng Q,et al.Dietary capsaicin and its anti-obesity potency:from mechanism to clinical implications[J].Bioscience Reports,2017,37(3):286．
• [8]Martel J,Ojcius D M,Chang C J,et al.Anti-obesogenic and antidiabetic effects of plants and mushrooms[J].Nature Reviews Endocrinology,2017,13(3):149-160．
• [9]DairamA,Fogel R,Daya S,et al.Antioxidant and iron-binding properties of curcumin,capsaicin,and S-allylcysteine reduce oxidative stress in rat brain homogenate[J].Journal of Agricultural and Food Chemistry,2008,56(9):3350-3356．
• [10]王宁，张正海，王立浩，等．不同栽培条件下辣椒果实辣椒素含量的分析与QTL定位[J]．中国蔬菜，2016(3):19-25．
• [11]常晓轲．干辣椒品种资源评价和栽培条件对辣椒素、辣椒红色素含量的影响[D]．泰安：山东农业大学，2014:17-18．
• [12]崔桂娟，谢秋涛，张群，等．辣椒中辣椒素提取方法与应用[J]．食品工业科技，2018,39(13):306-310．
• [13]高艺．辣椒中辣椒素提取分离纯化工艺的研究[D]．长沙：中南大学，2005:6-7．
• [14]丰金玉，周思杨，徐丹丹，等．超声波辅助提取辣椒素工艺技术研究[J]．中国农学通报，2016,32(11):43-48．
• [15]Dias A L B,Sergio C S A,Santos P,et al.Ultrasoundassisted extraction of bioactive compounds from dedo de mo9a pepper (Capsicum baccatum L.):effects on the vegetable matrix and mathematical modeling[J].Journal of Food Engineering,2017,198:36-44．
• [16]Keharom S,Mahachai R,Techawongstein S,et al.Optimization studies on ultrasonic assisted extraction of the capsaicinoids from sweet-to-superhot chilli samples using response surface methodology[J].InternationalFood ResearchJournal,2016,23(4):1676-1684．
• [17]庞敏，王远辉，刘茜．超声-微波协同辅助提取辣椒总碱的工艺优化[J]．食品与机械，2016,32(12):175-178,188．
• [18]Cienfuegos N E C,Santos P L,García A R,et al.Integrated process for purification of capsaicin using aqueous twophase systems based on ethanol[J].Food and Bioproducts Processing,2017,106:1-10．
• [19]Handoko L P,Variyana Y,Mahfud M.Studi Efektivitas Ekstraksi(capsaicin)Dari Cabai(Capsicum)Dengan Metode Sfme(solvent free microwave extraction)[J].JurnalTeknikITS,2017,6(2):385-387．
• [20]de Aguiar A C,Osorio-Tobón J F,Silva L P S,et al.Economic analysis of oleoresin production from malagueta peppers(Capsicum frutescens)by supercritical fluid extraction[J].The Journal of Supercritical Fluids,2018,133:86-93．
• [21]李晗，邵超，王新颖，等．超临界CO2萃取辣椒副产物中的辣椒碱[J]．现代食品，2019(15):186-189．
• [22]Zhou C,Ma D,Cao W,et al.Fast simultaneous determination of capsaicin,dihydrocapsaicin and nonivamide for detecting adulteration in edible and crude vegetable oils by UPLC-MS/MS[J].Food Additives&Contaminants:Part A,2018,1447-1452．
• [23]Ma F,Yang Q,Matthus B,et al.Simultaneous determination of capsaicin and dihydrocapsaicin for vegetable oil adulteration by immunoaffinity chromatography cleanup coupled with LC-MS/MS[J].JournalofChromatography B,2016,1021:137-144．
• [24]王穗萍，夏延斌，彭进，等．高效液相色谱法测定富含油脂辣椒制品中的辣椒素类物质[J]．分析试验室，2007(12):39-43．
• [25]赵琴，胡艺凡，许静，等．固相萃取-超高效液相色谱-串联质谱快速检测食用油和地沟油中辣椒素和二氢辣椒素[J]．分析科学学报，2014,30(6):777-782．
• [26]梁桂娟，寻思颖，张琼，等．LC-MS/MS法测定食用油中的辣椒素和二氢辣椒素[J]．中国酿造，2016,35(7):175-179．
• [27]Stoica R M,Moscovici M,Tomulescu C,et al.Extraction and analytical methods of capsaicinoids-a review[J].Biotechnologies,2016,20:93-98．
• [28]Do T L Z,Adam V,Zítka O.Determination of the content of capsaicin and dihydrocapsaicin in twelve varieties of chilli peppers using liquid chromatography with UV/VISdetection[C]//Mendel Net 2017,Proc.Int.PhD Students Conf.Brno,Mendel University in Brno,2017:861-866．
• [29]韦继雯，闫倩玲，周云波，等．中药材干辣椒中辣椒素和二氢辣椒素含量测定方法研究[J]．云南中医中药杂志，2018,39(7):76-78．
• [30]中国标准化委员会．食品安全国家标准食品添加剂辣椒油树脂：GB 28314-2012[S]．北京：中国标准出版社，2012．
• [31]厉志伟，王盛莉．高效液相色谱法测定辣椒中辣椒素、二氢辣椒素[J]．中国调味品，2017,42(11):123-126．
• [32]Potka-Wasylka J,Szczepańska N,de La Guardia M,et al.Modern trends in solid phase extraction:new sorbent media[J].TrAC Trends in Analytical Chemistry,2016,77:23-43.