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1.
气相色谱法测定食品中的香兰素   总被引:8,自引:0,他引:8  
香兰素(3-甲氧基-4-羟基苯甲醛)[1]是一种白至微黄色针状结晶粉,有香荚兰豆特有的香味,易溶于乙醇、乙醚、冰醋酸和热挥发油,沸点284~285℃,作为食品添加剂常用于冷饮、麦片、豆奶、糖果等食品.食品中香兰素的测定方法主要有薄层层析法[2],气相色谱法分析食品中的香兰素未见报道,本文对食品中的香兰素进行酸碱处理,多次萃取后用气相色谱法进行分析,样品回收率94.65%,变异系数0.12%,线性回归方程Y=(1.059e+04)X+(-17648.54) R=0.9977,结果令人满意.  相似文献   

2.
二极管阵列反相高效液相色谱法测定蜜饯中香兰素含量   总被引:1,自引:0,他引:1  
目的:建立二极管阵列反相高效液相色谱法测定蜜饯中香兰素含量的方法。方法:称取均质蜜饯样品到烧杯中,加入蒸馏水8,0℃水浴浸泡30 min,取出冷却至室温,转移到容量瓶中定容过滤,滤液待进样。采用XDB-C18色谱柱(5μm4,.6μm×150 mm),流动相为甲醇+乙酸铵(40+60v,/v),流速1.0 ml/min,二极管阵列检测器检测。结果:香兰素浓度在1.0μg/ml~30.0μg/ml范围内线性良好(r=0.9999,n=4),且峰形较好,回收率为102%,精密度RSD=2.3%;最低检出限为0.15μg/ml(以进量浓度计)。结论:二极管阵列反相高效液相色谱法测定蜜饯中香兰素含量的方法,定性准确、灵敏度高、回收率和重现性良好,操作快速,结果准确可靠。  相似文献   

3.
目的建立固相萃取-高效液相色谱法同时测定化妆品中香兰素和乙基香兰素的方法。方法样品经酸性乙腈提取后,采用固相萃取小柱HLB净化,洗脱液经氮气流吹干后用0.1%甲酸-乙腈(25∶75,V/V)溶液溶解,以0.1%甲酸-乙腈(25∶75,V/V)为流动相,经Shim-pack XR-ODSⅡ柱(75 mm×2.0 mm,2.2μm)分离后280 nm波长下检测,外标法定量。结果在0.02 mg/L~2.0 mg/L时线性相关系数0.999 0,香兰素和乙基香兰素的检出限分别为0.02 mg/kg和0.03 mg/kg,最低定量限分别为0.07 mg/kg和0.10 mg/kg,3个加标浓度的回收率为87.0%~98.2%,相对标准偏差为1.9%~4.6%。结论本法具有简便、快速、准确、干扰少的优点,可用于化妆品中香兰素和乙基香兰素的同时测定。  相似文献   

4.
食品添加剂的监测是食品卫生监测的重要内容。测定食品中香兰素的国际香兰素化学名:3-甲氧基-4-羟基苯甲醛,存在于香英兰豆、安息香膏中,有香草的特殊气味[1-2],是目前世界上生产量和使用量最大的人工合成香料,ADI值:0-10mg/kg(FAL/WHO,1994)[3].LD50:1580mg/kg,其在巧克力中的最大使用量为970mg/kg[4].目前尚无高效液相色谱法方法测定该食品中香兰素。故本实验研究以CH3OH:H2O=35:65为流动相,Reliasil C18为分析柱,使巧克力中香兰素很好的分离测定,样品中其它成分不干扰被测组分的准确定量[6-7],结果令人满意。  相似文献   

5.
食品添加剂的监测是食品卫生监测的重耍内容。食品中香兰素尚无国家标准方法(国标香兰素化学名:3-甲氧基-4-羟基苯甲醛)存在于香荚兰豆、安息香膏中,有香草的特殊气味[1-2],是目前世界上生产量和使用量最大的人工合成香料,ADI值0-10mg/kg(FAO/WHO,1994)[3]。LD50:1580mg/kg,其在巧克力中的最大使用量为970mg/kg,目前尚无高效液相色谱法方法测定食品中香兰素。故本实验以CH3OH:H2O=35:65为流动相,ReiasilC18为分析柱,使巧克力中香兰素很好的分离测定,样品中其它成分不干扰被测组份的准确定量,结果令人满意。1 材料与方法1.1 仪器及试剂 HP1100高效液相色谱仪:在线脱气机,四元泵,智能化柱相,紫外可变波长检测器(美国HP公司);HP3365化学工作站(美国HP公司);双重石英蒸馏水(上海亚荣),恒温水浴(上海)。 香兰素固体纯品,称取0.1000g于50ml烧杯中,以甲醇溶  相似文献   

6.
高效液相色谱法检测食品中香兰素的方法研究   总被引:2,自引:0,他引:2  
香兰素作为食品添加剂广泛用于麦片、糖果、豆奶、饮料等食品中,香兰素(又称3-甲氧基-4-羟基苯甲醛,番草醛)[1],是一种白至微黄色针状结晶粉,有香荚兰豆特有的香味,易溶于乙醇、乙醚、冰乙酸和热挥发油,沸点284-285℃,其测定方法主要有薄层层析法[2]、气相色谱法[3]等,测定时常须经酸、碱处理,有机溶剂萃取,手续繁琐。高效液相色谱法测定食品中的香兰素未见报道。本文对食品中香兰素的测定方法进行了研究,样品经过简单处理后,0.45μm滤膜过滤、用高效液相色谱法进行了研究,样品回收率94.99%…  相似文献   

7.
香兰素包括甲基香兰素(vanillin)和乙基香兰素(ethylvanillin),是食品中重要的香味添加剂,在糖果、糕点、饮料等食品中广泛使用。但是,大剂量使用香兰素对人体健康有害。1994年联合国粮农组织与世界卫生组织(FAO/WHO)规定甲基香兰素每日每公斤体重允许摄入量(ADI)为0~10mg/kg,1995年规定乙基香兰素的ADI为0—3mg/kg。在2000年欧盟专家委员会称,经多年的实验研究发现,大剂量使用香兰素可以导致头晕、恶心、呕吐、呼吸困难,甚至能够损伤肝、肾,对人体有较大危害,决定重新制定香兰素使用标准,进一步降低允许剂量。  相似文献   

8.
反相高效液相色谱法测定啤酒中香兰素   总被引:1,自引:0,他引:1  
笔者用高效液相色谱法测定啤酒中香兰素 ,以CH3 OH∶H2 O =35∶6 5为流动相 ,ReliasilC18为分析柱 ,使啤酒中香兰素很好的分离 ,样品中其他成分不干扰被测组分的准确定量 ,结果令人满意。1 资料与方法1 1 仪器及试剂HP110 0高效液相色谱仪 ;在线脱气机 ,四元泵 ,智能化柱相 ,紫外可变波长检测器 (美国HP公司 ) ;HP336 5化学工作站 (美国HP公司 ) ;双重石英蒸馏水 (上海亚荣 ) ;超声波清洗机 (上海 )。香兰素固体纯品 ,称取 0 10 0 0g于 5ml烧杯中 ,以甲醇溶解 ,并分别移入 10 0ml容量瓶中 ,定容至刻度 ,相当于香兰素 1 0 0mg/ml。…  相似文献   

9.
气相色谱法测定蜂王浆及制品中的10-羟基-2-癸烯酸   总被引:6,自引:0,他引:6  
目的 建立气相色谱法测定峰王浆及制品中的 10 -羟基 -2 -癸烯酸。 方法 采用H2 SO4-甲醇甲酯化 ,利用DB -WAX 0 .2 5mm× 0 .2 5 μm× 3 0m毛细管柱分离 ,FID检测器检测。  结果 在 0~ 5 0 μg/mL之间 ,线性关系良好、相关系数r =0 .9993 ,最低检出限为 0 .8μg/mL。  结论 用该气相色谱法测定结果可靠、重现性好 ,抗干扰强。测定基体成分比较复杂的蜂王浆样品 ,采用该气相色谱法检测结果可靠。  相似文献   

10.
目的 建立血清中敌敌畏浓度检测的气相色谱法,为临床诊断和监测提供定量依据.方法 取0.5 ml血清加乙酸乙酯2.0 ml充分震荡萃取,静置5 min,4000 r/min离心,取上清液,氮气吹干,50μl乙醇定容,取1.0μl进样玻璃填充柱,用氮磷检测器检测和气相色谱法分析.结果 血清中敌敌畏浓度在5.0~50.0 μg/ml范围内呈线性关系,回归方程y=804.13x-691.8,r=0.9992.最低检出浓度为2.0μg/ml,回收率为86.8%~94.5%,相对标准偏差(RSD)为4.6%~5.5%.日内、日间RSD分别为4.52%~5.21%和3.56%~5.52%.结论 该方法操作简便、分析快速,结果准确,适于临床的快速诊断敌敌畏中毒和量化评估治疗效果.  相似文献   

11.
HPLC法与香草醛比色法测定保健品中的人参皂甙   总被引:5,自引:0,他引:5  
〔目的〕应用高效液相色谱法和分光光度法分别同时检测保健食品中人参总皂甙的含量。〔方法〕高效液相色谱法采用短色谱柱 ,低乙晴体积分数 ,非线性梯度洗脱对 6种主要人参皂甙Rg1,Rb1,Re,Rb2 、Rc、Rd进行分析。〔结果〕方法回收率 95 .6 %~ 97.7% ,检出限 2 .2ng ,RSD =1.30 %~ 6 .90 %。分光光度法用大孔吸附树脂吸附人参总皂甙 ,经梯度洗脱处理 ,香草醛显色后测定人参总皂甙含量。方法回收率 :95 .6 %~ 10 7.4 % ,检出限 :1.2 5 μg,RSD =3.5 1%~ 4 .17%。两种方法测定人参总皂甙结果有显著性差异 (t=4 .5 1>t( 0 .0 5) =1.895 )。〔结论〕HPLC法适用于单个皂甙的测定 ,比色法适用于总皂甙含量的测定  相似文献   

12.
Owing to the presence of hemoglobin and polyunsaturated fatty acids, erythrocytes are a convenient model to understand membrane oxidative damage induced by various xenobiotic pro-oxidants. This study investigated the antioxidant activity of vanillin, a naturally occurring food-flavoring agent, against carbon tetrachloride (CCl(4))-induced erythrocyte damages in Wistar albino rats. A single injection of CCl(4) (1 ml/kg, intraperitoneally [i.p.]) caused a significant induction of oxidative damage as evidenced by increased thiobarbituric acid reactive substances, protein carbonyl levels and osmotic fragility accompanied with a significant decrease in Na(+)/K(+)-ATPase and Ca(2+)-ATPase activities. Furthermore, catalase and superoxide dismutase activities were significantly elevated, while glutathione levels, glutathione-S-transferase and glutathione peroxidase activities were markedly reduced in the erythrocytes of CCl(4)-treated rats. Pretreatment of rats with vanillin (150 mg/kg/day, i.p.) for 3 consecutive days before CCl(4) injection protected erythrocytes against the increase of lipid peroxidation and degradation of membrane proteins compared to CCl(4)-treated rats and exhibited marked prevention against CCl(4)-induced oxidative stress, alterations of membrane-bound enzymes as well as erythrocyte osmotic fragility. Our results suggest that vanillin plays a protective and curative role against the harmful effects of CCl(4) on erythrocytes, thus ensuring membrane cell integrity.  相似文献   

13.
4-(Bromomethyl) coumarins 1 have been reacted with vanillins, 2 and 2A to obtain the corresponding ethers 3 and 5. Ethers 3 have been reacted with ethyl cyanoacetate to obtain the unsaturated esters 4. Ethers 5 have been converted to the corresponding 4-(2'-benzo[b] furanyl) coumarins 6 by an intramolecular aldol condensation. Eight compounds have been screened for their anti-inflammatory activity. Out of these the 5,6-benzo-4-2'-benzo[b]furanyl) coumarin (6c) and the aryloxymethyl coumarin (4) with p-formyl group were found to be most active.  相似文献   

14.
Vanilla, being the world's most popular flavoring materials, finds extensive applications in food, beverages, perfumery and pharmaceutical industry. With the high demand and limited supply of vanilla pods and the continuing increase in their cost, numerous efforts of blending and adulteration in natural vanilla extracts have been reported. Thus, to ensure the quality of vanilla extracts and vanilla-containing products, it is important to develop techniques to verify their authenticity. Quantitatively, vanillin is the major compound present in the vanilla pods and the determination of vanillin is a vital consideration in natural vanilla extracts. This paper provides a comprehensive account of different extraction processes and chromatographic techniques applied for the separation, identification and determination of chemical constituents of vanilla. The review also provides an account of different methods applied for the quantification and the authentification of chemical constituents of vanilla extract. As the various properties of vanilla are attributed to its main constituent vanillin, its physico-chemical and bioactive properties have also been outlined.  相似文献   

15.
Vanilla, being the world's most popular flavoring materials, finds extensive applications in food, beverages, perfumery and pharmaceutical industry. With the high demand and limited supply of vanilla pods and the continuing increase in their cost, numerous efforts of blending and adulteration in natural vanilla extracts have been reported. Thus, to ensure the quality of vanilla extracts and vanilla-containing products, it is important to develop techniques to verify their authenticity. Quantitatively, vanillin is the major compound present in the vanilla pods and the determination of vanillin is a vital consideration in natural vanilla extracts. This paper provides a comprehensive account of different extraction processes and chromatographic techniques applied for the separation, identification and determination of chemical constituents of vanilla. The review also provides an account of different methods applied for the quantification and the authentification of chemical constituents of vanilla extract. As the various properties of vanilla are attributed to its main constituent vanillin, its physico-chemical and bioactive properties have also been outlined.  相似文献   

16.
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