高效液相色谱-蒸发光散射检测法同时测定固态食品中6种稀有糖  

Simultaneous determination of six rare sugars in solidfoods by high performance liquid chromatography-evaporative light-scattering detection

作　　者：刘宇 邢家溧 沈坚 毕晓丽 毛玲燕 徐晓蓉 张书芬 娄永江[1] 吴希 穆应花 LIU Yu;XING Jiali;SHEN Jian;BI Xiaoli;MAO Lingyan;XU Xiaorong;ZHANG Shufen;LOU Yongjiang;WU Xi;MU Yinghua(College of Food and Pharmaceutical Sciences,Ningbo University,Ningbo 315211,China;Ningbo Academy of Product and Food Quality Inspection(Ningbo Fibre Inspection Institute),Ningbo 315048,China)

机构地区：[1]宁波大学食品与药学学院,浙江宁波315211 [2]宁波市产品食品质量检验研究院(宁波市纤维检验所),浙江宁波315048

出　　处：《色谱》2023年第9期781-788,共8页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(32202060);浙江省自然科学基金项目(LZ23C200003);宁波市泛3315创新团队(2018B-18-C);宁波市高新精英创新团队(甬高科[2018]63号);宁波市重大科技攻关项目(2021ZDYF020179);宁波市甬江引才工程(2022A156G).

摘　　要：稀有糖在固态食品中的应用量与日俱增,引发了掺假、过量添加等食品安全问题,因此建立固态食品中稀有糖(阿洛酮糖、塔格糖、海藻糖、异麦芽酮糖、赤藓糖醇和甘露糖醇)的检测方法十分重要。本文基于高效液相色谱-蒸发光散射检测器,建立了一种同时检测固态食品中6种稀有糖的分析方法。选用Zorbax Original NH_(2)色谱柱(250 mm×4.6 mm,5μm)进行分离,流动相为乙腈-水(80∶20,v/v),流速梯度洗脱。蒸发光散射检测系统的漂移管温度设置为50℃,雾化器载气为高纯氮,载气流速为1.0 mL/min,压力为275.79 kPa,增益值为3。样品经25 mL水提取,振荡涡旋10 min,分别加入200μL的乙酸锌溶液和200μL的亚铁氰化钾溶液净化,4500 r/min离心10 min,取上清液1 mL,过0.22μm水相滤膜,待上机分析。6种稀有糖在各自范围内线性关系良好,决定系数(R^(2))均>0.9985,方法的检出限为0.02~0.60 g/100 g。以空白固态食品样品为基质,在3种加标水平下,6种稀有糖的回收率为92.6%~103.2%,相对标准偏差为0.7%~4.4%。将该方法用于分析实际固态食品样品中6种稀有糖的含量,结果显示,实际成分和食品标签所示基本一致。本研究建立的方法前处理操作简单,重复性好,方法快速、灵敏、准确,可应用于日常监测固态食品中6种稀有糖的含量,同时为稀有糖的检测提供了一种具有广阔前景的技术手段。Excessive sugar consumption is associated with metabolic health problems.Rare sugars are gradually being used as substitutes for sugar,and their consumption is increasing daily,raising food-safety issues such as false advertising,adulteration,and overdosing.The determination of rare-sugar compounds has attracted considerable attention in recent years.However,no standard method for the simultaneous determination of six rare sugars(allulose,tagatose,trehalose,isomaltulose,erythritol,and mannitol)in solid foods is available.Therefore,establishing a suitable analytical method for these sugars is necessary.In this study,high performance liquid chromatography coupled with evaporative light-scattering detection was used to determine rare sugars in solid foods.The optimum chromatographic and detector conditions were determined by evaluating the instrument parameters.Analysis was carried out on a Zorbax Original NH 2 column(250 mm×4.6 mm,5μm)via flow-rate gradient elution(0-15 min,1.0 mL/min;15-18 min,1.0-2.0 mL/min;18-25 min,2.0 mL/min)with acetonitrile-water(80∶20,v/v)as the mobile phase.Sharp and symmetric chromatographic peaks were obtained under these conditions.The resolutions for all the six rare sugars were greater than 1.5.Optimization of the evaporative light-scattering detector was extremely important to the responses of the rare-sugar compounds.The two most significant parameters were the nebulizer carrier gas flow rate and drift tube temperature.The detection system was operated under the following conditions:the drift tube temperature was set to 50℃,the nebulizer carrier gas was high-purity nitrogen,the carrier gas flow rate was 1.0 mL/min,the nitrogen pressure was regulated to 275.79 kPa,and the gain factor was set to 3.The sample was extracted with 25 mL of water,shaken and vortexed for 10 min,purified with 200μL of zinc acetate solution and 200μL of potassium ferricyanide solution,and centrifuged at 4500 r/min for 10 min.Next,1 mL of the supernatant was passed through a 0.22μm aqueous-phase filte

关 键 词：高效液相色谱 蒸发光散射检测器 稀有糖 固态食品 

分 类 号：O658[理学—分析化学]