反相高效液相色谱法测定饮料中咖啡因含量

目的建立一种简单流动相洗脱的反相高效液相色谱法快速测定饮料中咖啡因含量。方法以甲醇-水-乙酸为流动相,对饮料进行简单的过滤处理后直接进样测定。结果标准曲线的回归方程为y=52.54635x+47.46411,相关系数r=0.99996;测定咖啡因保留时间的标准偏差为0.087 min,RSD为1.41%;浓度的标准偏差为2.22 mg/L,RSD为1.98%;测定结果的总体回收率在97.5%~98.1%之间;加标回收率在92.2%~95.9%之间。结论采用本法测定饮料中的咖啡因含量,具有结果准确、样品处理方法简便、流动相组成简单等优点,适合饮料中咖啡因的测定。     

反相高效液相色谱法测定饮料中的咖啡因

[目的 ]精确测定咖啡因在饮料中的含量 ,建立测定饮料中咖啡因含量的RP HPLC法的最佳工作条件。 [方法 ]色谱柱为WatersSymmetryRP18:15 0× 3 9mm (5 μm ) ;流动相为A为 0 0 2M乙酸铵 ,B为甲醇 ;流速为 0 7ml/min ;DAD检测波长 2 0 7nm。 [结果 ]本法操作简便、准确、线性关系良好 ,相对标准偏差小于 1% ,加标回收率为 90 1%～10 1 0 %。　 [结论 ]与现行国标方法相比 ,通过优化了的色谱条件 ,节省了贵重的有机溶剂 ,提高了测定灵敏度及检出范围。     

高效液相色谱法同时测定多维营养片中维生素B6、烟酰胺和泛酸钙

目的:建立同时测定维生素补充剂中维生素B6、烟酰胺和泛酸钙含量的液相色谱法。方法:样品在提取液中经超声提取和水浴加热溶解后,以0.05 mol/L磷酸二氢钾溶液(pH=3.00±0.05)-甲醇-乙腈(90:6:4)为流动相,经In-ertsil PH-3苯基柱分离,在波长210 nm处检测,外标法定量。结果:维生素B6、泛酸钙和烟酰胺分别在0.0024~0.060 mg/ml(r=0.9999)、0.0080~0.20 mg/ml(r=0.9999)、0.017~0.42 mg/ml(r=0.9999)浓度范围内呈良好的线性关系,维生素B6、泛酸钙和烟酰胺的平均回收率分别为97.2%、99.9%、101.2%。结论:该方法简便、准确、重现性好,适用维生素类保健食品的日常质量控制。     

反相高效液相色谱法测定巧克力中咖啡因

咖啡因又名咖啡碱 ,化学名 1,3,7—三甲基黄嘌呤。具有提神作用 ,但易上瘾[1] 。国标法规定了咖啡因的测定方法 ,但本实验室应用该法分别以ＨｙｐｅｒｓｉｌＢＤＳＣ18(大连依利特 )及Ｒｅ ｌｉａｓｉｌＣ18(ＡＩＣＨＲＯＭ公司 )两根色谱柱按照方法提供的流动相组成 [ＣＨ3 Ｏ     

高效液相色谱法同时测定元素多维片中5种水溶性维生素

目的:建立反相高效液相色谱法同时测定多维元素片中烟酸、维生素B1、维生素B6、烟酰胺和维生素B2的方法。方法:Phenomenex C18色谱柱(150 mm×4.6 mm,5μm);0.05 mol/L磷酸二氢钾为流动相A,乙腈为流动相B,梯度洗脱;柱温:35℃;流速:0.8 ml/min;检测波长:265 nm。结果:烟酸、维生素B1、维生素B6、烟酰胺和维生素B2的线性范围分别为6.15~393.76μg/ml、6.44~412.32μg/ml、6.85~438.24μg/ml、6.46~413.12μg/ml和3.26~52.15μg/ml。平均回收率分别为:烟酸104.8%、维生素B1 99.7%、维生素B6 95.3%、烟酰胺103.4%和维生素B296.9%。结论:本方法同时测定5种维生素,具有快速、简便、准确的特点。     

高效液相色谱法测定饮料中的咖啡因

目前饮料中咖啡因的测定方法有薄层色谱法、紫外分光光度法、气相色谱法和高效液相色谱法.其中用高效液相色谱法测定饮料中的咖啡因有两种方法.一种为饮料中糖精钠、咖啡因、苯甲酸的高效液相色谱测定方法[1];另一种饮料中咖啡因的测定方法[2].本文对上述两种方法用色谱柱C18分别进行了改进,并获得满意的结果.现把两种方法中不同的实验条件与结果叙述如下.     

高效液相色谱法快速测定饮料中咖啡因,山梨酸,苯甲酸和糖精钠

高效液相色谱法快速测定饮料中咖啡因、山梨酸、苯甲酸和糖精钠辽宁省沈阳市卫生防疫站（１１００３１）黄贞子张田萃贾薇目前饮料中咖啡因、山梨酸、苯甲酸和糖精钠的常用测定方法有分光光度法［１，２］、气相色谱法［１～３］、高效液相色谱法（ＨＰＬＣ）［４～６］。...     

反相高效液相色谱法同时测定糖精钠、咖啡因,苯甲酸、山梨酸

各种食品添加剂的应用日益广泛,并且同一种食品中同时添加多种添加剂,甜味剂、防腐剂及具有特殊生理作用的咖啡因等。然而国际检验方法中一次只能检测一种或两种添加剂[1-3],为测定多种成分不得不频繁改变仪器条件,以达到分析不同组分的目的。这给分析工作者的检测工作带来很多麻烦。为此本实验研究将糖精钠、咖啡因、苯甲酸、山梨酸四种食品添加剂一次进样同时分析,节省了分析时间,省去了配制多种流动相的不便,同时提高了工作效率,经过对可乐饮料、功能性保健饮料及茶的测定,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,智能化柱箱,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）;双重石蒸馏水器（上海亚荣）;超声波清洗机（上海）。糖精钠、山梨酸、苯甲酸标准液1.00mg/ml均由中国标准技术研究中心提供。甲醇、乙腈为HPLC级试剂;无水KH2PO41     

同时测定保健食品中褪黑素和维生素B6的高效液相色谱方法研究

目的 建立了一种快速同时分析保健食品中褪黑素和维生素B6的高效液相色谱法.方法 样品用0.1％磷酸提取,离心后取上清液进样,经甲醇-水(v/v,55∶45)洗脱,反相C18柱分离,紫外检测器在278 nm、290 nm波长处分别测定褪黑素和维生素B6的含量.结果 褪黑素和维生素B6测定的线性范围分别是1.0 ～160.0 μg/ml和1.0～100.0μg/ml,最低检出限分别为0.14 μg/ml和0.10μg/ml,标准溶液测定的保留时间和峰面积的相对标准偏差(relative standard deviation,RSDs)分别为5.18％和1.31％(褪黑素),2.84％和1.26％(维生素B6).将所建立的方法用于保健食品样品的测定,取得了较为满意的效果,样品测定的RSDs分别为2.01％(褪黑素)和1.87％(维生素B6),平均加标回收率分别是92.2％～104.3％(褪黑素)和94.5％～110.0％(维生素B6),将本法测定样品的结果与标准方法比较,相对误差为-1.94％～1.01％(褪黑素)和-5.45％4.35％(维生素B6).结论 该法快速准确,10 min内可完成一次分析,适用于保健食品中褪黑素和维生素B6含量的快速同时分析.     

高效液相色谱法同时测定化妆品中地塞米松和泼尼松

目的：建立高效液相色谱法测定化妆品中地塞米松和泼尼松的方法。方法：醋酸氟氢可的松为内标，乙腈-水-乙酸铵溶液为流动相，甾体激素经C18色谱柱反相液相色谱分离紫外检测。结果：被测两组分浓度在5—200μg／ml范围呈良好线性关系，回收率分别为95．9％和94．7％，相对标准偏差分别为4．55％和4．11％。结论：本方法准确可靠，适合化妆品中地塞米松及泼尼松的含量测定。     

高效液相色谱法同时测定尿液中溴敌隆和溴鼠灵的方法研究

目的:建立反相高效液相色谱法同时快速检测尿液中的溴敌隆、溴鼠灵的分析方法。方法:尿样经乙酸乙酯提取过滤后直接进样,以甲醇-1%甲酸(90:10,V/V)为流动相,流速1.0 ml/min,经ODS-C18色谱柱(150 mm×4.6 mmi.d,5.0μm)40℃分离,在波长265 nm处检测。结果:分离测定过程在10 min之内完成,保留时间分别为溴敌隆3.770 min、溴鼠灵8.110 min。溴敌隆、溴鼠灵线性范围均为0.02～50.0μg/ml,最低检出量为0.16 ng。低、中、高3个浓度水平的样品加标平均回收率为86.0%～109.0%,保留时间与峰面积的日内和日间相对标准偏差分别<1%和<5%。结论:本方法简便、快速、稳定、准确,实用性强,满足中毒应急检测及临床治疗的需要。     

Simultaneous determination of retinol, carotenoids and tocopherols in human serum by high pressure liquid chromatography

The determination of serum vitamins having antioxidant properties has gained in importance in recent years. This is mainly due to the observation that an inverse correlation exists between blood levels of these vitamins, including retinol, carotenoids and tocopherol, and diet-related chronic diseases such as coronary heart disease and cancers. This laboratory has been carrying out a series of studies into the nutritional and analytical aspects of retinol and carotenoids. A simple reversed-phase HPLC method has been developed in an effort to improve methodologies for the separation and quantitation of carotenoids and retinol in foods and biological specimens, especially blood serum. As an extension to these studies, trials were carried out to determine the feasibility of analysing tocopherols using the same chromatographic procedure. With the addition of another detector wavelength, the same procedure detected and quantitated 3 major tocopherols simultaneously with retinol and five carotenoids. Within-day and between-day precision of the procedure was satisfactory. Trials carried out were able to improve recovery of the vitamins. Experiments conducted also showed that the addition of ascorbic acid to the extracting ethanol was beneficial for the analytical procedure. The presence of peroxide in ethyl acetate used in the chromatography mobile phase caused drastic destruction to the vitamins analysed. The addition of ascorbic acid during sample preparation was able to inhibit this destruction. The method was used for the analysis of sera from 65 apparently healthy Malaysians with a mean age of 52.8 years (range 24-76 years). Mean retinol concentration of the group was 69.8 ± 18.8 mg/dl. The mean β-carotene concentration of the subjects studied was 33.8 ± 24.3 mg/dl, while the mean total carotenoid concentration was 180.2 ± 3.0 mg/dl. The most abundant carotenoid in the serum samples studied was lutein, comprising about one-third of all carotenoids quantitated. The concentrations of δ- and γ-tocopherols in the serum samples studied were too low to be identified with certainty and quantitated accurately. The mean α-tocopherol level was 1840 ± 528 μg/dl. For retinol, α-tocopherol and most of the carotenoids determined, there was no statistically significant difference in the mean levels between male and female subjects as well as among the three different ethnic groups. Results obtained in this study were very similar to those previously reported by this laboratory. It is hoped that more data on the serum concentrations of these vitamins can become available for various population groups, including during various disease conditions.     

反相高效液相色谱梯度洗脱法测定乳饮料中9种食品添加剂

目的:建立反相高效液相色谱法同时测定乳饮料中9种食品添加剂的分析方法。方法:样品经甲醇处理后采用Gemini C18柱(250 mm×4.6 mm×5μm)以乙腈-三氟乙酸-乙酸铵为流动相进行梯度洗脱分离,紫外检测器测定,外标法定量。检测波长为210 nm,柱温30℃。结果:安赛蜜、糖精、咖啡因、阿斯巴甜、苯甲酸、山梨酸、脱氢乙酸和纽甜在5.0 mg/L～100.0 mg/L范围均具有良好的线性,甜菊糖苷在10.0 mg/L～200.0 mg/L范围具有良好的线性,9种待测物的回收率在93.2%～103.3%范围,RSD均小于6.0%,最低定量检出限在1.0 mg/kg～10 mg/kg范围。结论:该方法前处理简单,梯度洗脱分离效果和重现性好,具有快速、灵敏、简便、准确等优点,能满足实际工作的需要。     

Simultaneous determination of retinol, tocopherols, carotenes and lycopene in plasma by means of high-performance liquid chromatography on reversed phase.

The determination of the vitamins A and E as well as of carotenes and lycopene is important for studies of cardiovascular diseases and cancer. A method for laboratory routine is reported to separate simultaneously retinol, tocopherols, alpha- and beta-carotene, lycopene and beta-cryptoxanthin in human plasma or serum by HPLC on reversed phase starting from one extract. Two detectors with programmable wavelength are used sequentially, a spectrophotometer for the detection of the carotenoids in the visible region and a fluorometer for the assay of retinol and the tocopherols.     

固相萃取结合高效液相色谱测定鸡肉中10种磺胺类药物残留

目的:建立鸡肉中10种磺胺类药物残留的HPLC测定方法。方法:鸡肉经过甲醇提取,正己烷脱脂,SLW固相萃取柱净化,用HPLC法测定鸡肉中10种磺胺类药物的含量。结果:当鸡肉样品添加10种磺胺类药物为0.05~0.2 mg/kg时,方法回收率为67.4%~95.6%,变异系数为4.8%~11.5%,10种磺胺类药物最低检出浓度为0.01 mg/g。结论:以HPLC法测定鸡肉中10种磺胺类药物残留,操作简便、定量准确可靠。     

Simultaneous determination of alpha-tocopherol and retinol in plasma or red cells by high pressure liquid chromatography.

This paper describes a rapid, microprocedure for the simultaneous determination of alpha-tocopherol (vitamin E) and retinol (vitamin A) in plasma, and of alpha-tocopherol alone in red cells since cells do not contain retinol. A total lipid extract from 0.1 ml plasma or 0.125 ml red cells and containing internal standards of alpha-tocopheryl acetate and retinyl acetates is injected onto a high pressure liquid chromatography with a reverse phase column developed with methanol-water. An ultraviolet detector with 280-nm filter is used. The chromatogram is complete in 8 min and the alpha-tocopherol and retinol are quantitated by the peak height ratio method. Comparison of results with both plasma and red cells gave excellent agreement with conventional methods for these vitamins. The procedure should be particularly useful for clinical studies and nutrition surveys.     

茶叶及茶饮料中儿茶素和咖啡因的多组分HPLC分析方法

目的　建立茶叶及茶饮料中儿茶素和咖啡因多组分HPLC测定方法。方法　以水 -乙醇 (3∶7)为提取剂 ,超声提取 ,提取液离心后 ,采用C1 8柱分离 ,HPLC- UV检测。以 0 . 1%H3PO4 的甲醇溶液为流动相A ,0 .1%H3PO4 的水溶液为流动相B ,进行梯度洗脱 ,流速为 1ml min,检测波长为 2 10nm。结果　在给定的浓度范围内 ,各儿茶素组分和咖啡因的峰面积与其相应浓度呈现良好的线性相关 ,r>0. 999。添加已知儿茶素含量的茶粉回收试验结果显示 ,各组分儿茶素及咖啡因的平均回收率为 6 1. 7%～ 117. 4 % ,相对标准差 <10 %。结论　本方法分离度好 ,灵敏度高 ,准确快速 ,为研究儿茶素在机体内的吸收利用提供了可靠手段。     

保健品中芍药苷含量的二极管阵列反相高效液相色谱测定法

目的建立用反相高效液相色谱测定保健食品、保健用品中功效成分芍药苷的方法。方法样品中芍药苷经甲醇或水提取、C18反相柱分离,在波长232 nm处检测。结果方法的回收率为96.3%～100.4%,RSD为1.4%～1.7%。结论该方法简便快速,准确可靠,可用于各类保健品中芍药苷含量的测定。