【作者】 刘源；

【导师】 别小妹；

【作者基本信息】 南京农业大学 ， 工程硕士（专业学位）， 2015， 硕士

【摘要】 糖尿病是一种由胰岛缺陷引起的代谢性内分泌疾病,治疗方式包括饮食、运动、药物等多方面,一般以药物控制为主。随着经济的发展,生活水平的提高,大众对于一些具有辅助降糖作用的食品热衷度越来越高。目前,常见降糖食品主要有两大类:一是天然的含有多糖成分和植物膳食纤维的食品,如南瓜、魔芋等;二是经注册批准生产的降糖保健品,如功能饮料、各种口服降糖制剂等。我国食品法规定:保健食品属于食品范畴,对人体机能有一定的调节作用,但不以治疗疾病为目的。由此可见,辅助降糖的保健品是不允许含有化学活性物质的。然而,近年来一些生产企业为获得高额利润,在生产中非法添加化学降糖药,夸大治疗效果。一旦消费者购买、服用此类含有非法添加成分的保健食品,会引起血糖过低、昏迷甚至危及生命。本文研究的降糖保健食品为拮糖胶囊,是一种经国家食药监局批准生产的功能性降糖类保健食品。目前,该产品主要通过药店、商场、网络等渠道销售,使用人群广泛。本文首次对拮糖胶嚢开展非法添加检测研究,根据产品的适用范围,采用三氯甲烷超声提取,以三氯甲烷-石油醚(30～60℃)-甲醇-冰醋酸(10:15:1:1)为展开剂;点样量5μL的TLC快速鉴定检测方法,可以实现对拮糖胶囊非法添加物的快速专项检查及其可能含有的添加物进行初步筛选,确定化学物质品种范围为格列本脲、格列奇特、格列吡嗪三种物质。由于样品配方所含成分较复杂,单独使用TLC法检测,干扰较大,定性依据不足。为避免假阳性的现象,使用二极管阵列检测对样品同时进行光谱、色谱扫描,通过色谱峰纯度及三维图谱的比较,确定样品中含有的非法添加物为格列苯脲。在定性分析同时,对样品含有的添加物采用高效液相色谱进行定量检测,建立了 HPLC法测定糖胶囊中格列苯脲含量,并完成一系列的方法学考察,结果为每粒拮糖胶嚢含格列苯脲6.21mg,对患者安全使用该产品提供了参考。本文建立的TLC结合HPLC定性、定量检测方法,在0.5125-3.0750μg/ml范围内线性关系良好,平均加样回收率为97.29%,精密度RSD为0.12%(n=6),便捷、可靠、易于操作、灵敏度高、专属性强,有望用于功能性降糖保健食品拮糖胶囊非法添加物的快速筛查,对其产品质量控制具有指导意义。更多还原

【Abstract】 Diabetes is a kind of endocrine metabolic disease caused by the pancreatic defect.The treatment includes dieting,exercises,medication and so on.Among them,medication remains the main way.With the development of the economy and the improvement of human’s living standard,some health food with a consequent effect of adjuvant therapy has become increasingly popular.At present,the common hypoglycemic food contains two major categories,firstly,natural ingredients and plant foods containing dietary fiber polysaccharides,such as pumpkin,konjac,etc;secondly,the health care products glucose registered and approved,such as functional beverages,a variety of oral hypoglycemic agents and so on.According to the management of the relevant laws of health food in our country,health food belonging to food,should have certain body function regulating effect,while should not aim at treating disease,which is different from drugs.Therefore,regulating blood sugar health food definitely should not contain chemical ingredients.However,in recent years,in order to obtain high profits,some producers illegally added hypoglycemic agents into the health food,exaggerated treatment effects and attract consumers with false advertisement.Once consumers buy and take these health food containing illegal addion,low blood sugar,coma or even life-threatening may happen.Jietang capsules,one kind of hypoglycemic health food approved by China Food and Drug Administration was studied in this paper.Currently,the products are mainly sold in pharmacies,shopping centers,networks,and other sales channels,with extensive use.The detection of illegal additives in Jietang Capsules was carried out in this paper for the first time.According to the indication,chloroform was used for ultrasonic extraction,and the detection method for rapid identification of TLC was chloroform-petroleum ether(30～60 ℃)-methanol-acetic acid(V:V=10:15:1:1)as the eluent with the spotting amount being 5μL.This method can realize rapid special inspection and find the potential additives preliminarily.Glibenclamide,gliclazide,glipizide were determined to be the three substances in the range of chemicals.Since the sample recipe ingredients is rather complex,TLC used alone,interfers and lacks qualitative basis.To avoid being false positive,DAD was used for the spectroscopy and chromatography scanning simultaneously.By comparing the chrom atographic peak purity and three-dimensional map,illegal additive contained in the sample was determined to be glyburide.Besides qualitative analysis,HPLC quantitative detection of additives was carried out.HPLC method was established and a series of methodological study was carried out for the determination of the content of glibenclamide in Jietang capsules.The result is each Jietang capsule containing 6.21 mg of glyburide which provi des a reference for patients’safety.The established HPLC-TLC combined qualitative and quantitative detection meth od has good linear relationship in the range of 0.5125-3.0750μg/ml.The average recovery rate was 97.29%and the RSD was 0.12%(n=6).The method was convenient,reliable,easily operated and has high sensitivity and good specificity,which shows expect for rapid screening of illegal additives in the functional health food,Jietang capsules and is instructive for its product quality control.更多还原