在线固相萃取-液相色谱法测定食品中4种类胡萝卜素含量  

Determination of 4 kinds of carotenoids in foodstuffs by online solid phase extraction-liquid chromatography

作　　者：周锋杰 夏钰 张艳海 ZHOU Feng-Jie;XIA-Yu;ZHANG Yan-Hai(Suzhou Agricultural Products Safety and Quality Inspection Center,Suzhou 215104,China;NanoChrom Analytical Technology(Suzhou)Co.,Ltd.,Suzhou 215000,China)

机构地区：[1]苏州市农产品质量安全监测中心,苏州215104 [2]纳谱分析技术(苏州)有限公司,苏州215000

出　　处：《食品安全质量检测学报》2025年第4期209-214,共6页Journal of Food Safety and Quality

摘　　要：目的建立在线固相萃取-液相色谱法(online solid phase extraction-liquid chromatography,online SPE-LC)同时测定婴幼儿配方乳粉和天然食品中叶黄素、玉米黄质、α-胡萝卜素和β-胡萝卜素含量的方法。方法样品采用浓度为50%氢氧化钾溶液在70℃下皂化15 min,皂化液以70%乙醇定容,高速离心后取上清液直接上机分析。选择聚苯乙烯-二乙烯基苯基质的SelectCore PSS色谱柱作为online SPE柱,采用80%甲醇-水作为初始上样溶剂,乙腈/甲基叔丁基醚作为清洗溶剂。采用ChromCore C30(4.6 mm×250 mm,3μm)作为分析柱,乙腈-甲醇(26:74,V:V,含0.4 g/L抗坏血酸)与甲基叔丁基醚作为流动相,梯度洗脱,流速为1.0 mL/min,检测波长为450 nm。结果婴幼儿配方乳粉和天然食品中4个目标物分离良好,所有目标物的线性相关系数r>0.9999,叶黄素、玉米黄质及α-胡萝卜素、β-胡萝卜素的方法定量限分别为0.77、0.72、0.94、1.40μg/100 g,婴幼儿配方乳粉基质加标平均回收率分别为99.76%、103.51%、99.16%和97.92%;方法重复性的相对标准偏差小于2.5%。结论该方法快速、可靠及重复性良好,可满足食品中叶黄素、玉米黄质和α-胡萝卜素、β-胡萝卜素的定量要求,可被应用于实际样品的检测中。Objective To develop a method for the simultaneous determination of lutein,zeaxanthin,α-carotene,andβ-carotene in infant formula milk powder and natural foods by online solid phase extraction-liquid chromatography(online SPE-LC).Methods Samples were saponified with 50%potassium hydroxide solution at 70℃for 15 min.Saponified solution was diluted with 70%ethanol,and after high-speed centrifugation,the supernatant was directly analyzed.A styrene-divinylbenzene copolymer-based SelectCore PSS-packed chromatographic column was chosen as the online SPE column,using 80%methanol-water as the initial loading solvent and acetonitrile/methyl tert-butyl ether as the washing solvent.A ChromCore C30 column(4.6 mm×250 mm,3μm)was used as the analytical column,with acetonitrile-methanol(26:74,V:V,0.4 g/L of ascorbic acid)and methyl tert-butyl ether as the mobile phase for gradient elution.The flow rate was 1.0 mL/min,and the detection wavelength was 450 nm.Results The 4 target analytes in infant formula milk powder and natural foods were well separated.Linear correlation coefficients for all target analytes were greater than 0.9999.The limit of quantification of method for lutein,zeaxanthin,α-carotene,andβ-carotene were 0.77,0.72,0.94,and 1.40μg/100 g,respectively.Average recovery rates of infant formula milk powder were 99.76%,103.51%,99.16%,and 97.92%,respectively.The relative standard deviations of method repeatability for all the analytes were less than 2.5%.Conclusion This method is accurate,reliable,and reproducible and can meet the quantitative requirements of lutein,zeaxanthin,andα-carotene,β-carotene in foodstuffs.It can be applied to the determination of real samples.

关 键 词：胡萝卜素 叶黄素 玉米黄素 婴幼儿配方乳粉 天然食品 在线固相萃取-液相色谱法 

分 类 号：TS2[轻工技术与工程—食品科学与工程]