高效液相色谱法测定面粉中的过氧化苯甲酰

主要从烘焙品质和蒸煮品质方面综述了小麦蛋白质含量、结构和组成与面制品品质的关系，以期为面制品品质的改善提供理论依据，并对小麦蛋白质的研究发展作了进一步的展望。研究表明：麦谷蛋白大聚合体含量是决定面包烘焙品质的一个重要品质指标。作为品质代表指标优于面筋和蛋白质含量。今后应加强同种小麦胚乳结构中蛋白质含量和质量与面制品品质关系的研究，以及清蛋白和球蛋白对面制品品质影响的研究；     

高效液相色谱法同时测定食品中多种添加剂

为建立一种应用高效液相色谱法同时测定新红、胭脂红、糖精钠、日落黄、苯甲酸、山梨酸、香兰素、亮蓝、赤藓红9种食品添加剂的分析方法,采用梯度洗脱技术,以C18柱(250 mm×4.6 mm,5μm)为分离柱,以甲醇-0.02 mol/L乙酸铵(p H 5.77)-乙腈(乙酸铵溶液与乙腈体积比8.25∶1)为流动相,用紫外检测器在波长230nm处检测饮料、酱菜等样品。样品经过处理后直接进样,1次进样分析可在13 min内实现基线分离。该方法的线性相关系数范围为0.9979~0.9998,检测限0.025~2.0μg/m L,平均回收率在83.4%~111.4%之间,相对标准偏差(RSD)5.5%。该方法灵敏度高,重现性好,操作方便、快速,是检测食品添加剂的有效方法。     

高效液相色谱法快速测定红富士苹果渣中的6种多酚

为了建立快速检测苹果多酚的反相高效液相色谱法,通过选择合适的流动相,采用梯度洗脱并且调整进样量及流速,最终达到了很好的分离效果。该方法能在20min内检测出苹果渣中的6种酸性酚和黄酮类物质,检测限为0.008～0.088μg/g,样品加标回收率均>90%,相对标准偏差为1.3%～2.4%,说明该方法准确可靠。用该方法检测了红富士苹果渣中多酚的含量,实验表明,样品中的多酚类物质包括绿原酸、儿茶素、表儿茶素、芦丁、根皮苷等。     

高效液相色谱法测定口罩中5种荧光增白剂

建立了同时测定口罩中5种荧光增白剂(FWAs)的高效液相色谱检测方法。口罩样品经乙腈-N,N-二甲基甲酰胺-水(3∶3∶7,v/v)超声提取,提取液由十八烷基键合硅胶(C₁₈)和氨基硅胶混合吸附剂净化,以ODS Hypersil(2.5μm×4.6 mm×250 mm)C18色谱柱进行分析,以乙腈和水作为流动相梯度洗脱,外标法定量。5种FWAs在0.005～1.000 mg/L内呈良好的线性关系,相关系数(r)为0.983 2～0.999 9。样品的平均加标回收率为71.60%～102.87%,相对标准偏差(RSD)为2.3%～8.5%(n=3)。该方法灵敏度高,精密度好,准确度高,适用于不同口罩中FWAs的测定。     

QuEChERS-高效液相色谱法同时测定苹果中7种苯甲酰脲类农药残留

摘 要：目的 建立一种QuEChERS-高效液相色谱法(high performance liquid chromatography, HPLC)同时测定苹果中除虫脲、灭幼脲、杀铃脲、氟铃脲、氟苯脲、氟虫脲和氟啶脲7种苯甲酰脲类农药残留量的分析方法。方法 样品加1%冰乙酸-乙腈（体积比,冰乙酸：乙腈=1:99）、氯化钠、无水乙酸钠、无水硫酸镁提取,离心,上清液经无水硫酸镁和N-丙基乙二胺（PSA）净化后离心,取上清液氮气吹干,残渣经流动相溶解后,过0.22 μm滤膜,高效液相色谱仪分析。结果 本方法7种组分在0.0 μg/mL ~ 2.0 μg/mL范围内具有良好的线性关系,相关系数大于0.9995,加标回收率为81.7%~116.9%,相对标准偏差为0.1%~2.0%。检出限在0.007~0.017 g/kg范围,定量限在0.02~0.07 g/kg范围。结论 该方法操作简单,结果准确,适合苹果中除虫脲、灭幼脲、杀铃脲、氟铃脲、氟苯脲、氟虫脲和氟啶脲的检测。     

高效液相色谱法同时测定酱腌菜中15种 食品添加剂的含量

目的建立同时测定酱腌菜中15种食品添加剂的高效液相色谱法。方法样品经过提取净化后,在优化的梯度洗脱条件下分离,二极管阵列检测器进行检测。结果 15种食品添加剂在给定的浓度范围内各添加剂的浓度与峰面积具有良好的线性关系,相关系数(r)在0.9991~0.9998之间。该方法检出限为3.0~6.5 mg/kg,加标回收率为86.4%~103.4%,相对标准偏差为2.48%~8.10%。结论该方法回收率高、精密度高、准确度高、重现性好,是测定酱腌菜中15种添加剂的有效方法。     

高效液相色谱法测定奶粉中唾液酸的含量

利用酸水解法可释放出奶粉中的蛋白结合态唾液酸,以邻苯二氨盐酸盐为衍生化试剂,80℃水浴中衍生40min,采用Symmetry C18柱（250 mm×4.6mm,5цm）,流动相为1.0%的四氢呋喃水溶液（含0.2%磷酸）-乙腈（92：8）,流速为1.0mL/min,紫外检测波长227nm。结果表明,唾液酸在质量浓度为20～500mg/L范围内线性良好,平均回收率为96.8%。该方法具有灵敏度高,重复性好等特点,可准确测定奶粉中唾液酸的质量浓度。     

高效液相色谱法测定饮料中防腐剂和甜味剂

建立了高效液相色谱-示差折光检测器法同时测定碳酸饮料中苯甲酸、山梨酸、糖精钠、甜蜜素的分析方法,考察了流动相配比、缓冲溶液的浓度、柱温、检测器的温度及灵敏度设置对测定的影响,确定了最佳色谱条件:Novo pak-C18柱,示差折光检测器(RID),流动相为甲醇-0.010mol/L乙酸铵溶液(3:97,V/V),等度洗脱方式,柱温及RID检测器温度30℃,RID检测器灵敏度设置64.结果显示,线性范围为2.0～200μg/ml,相关系数为0.9995～0.9999,检出限依次为0.2、0.2、0.2、1.3μg/ml,相对标准偏差2.1%～3.5%,平均回收率89.0%～104.5%,实现了min内对碳酸饮料中苯甲酸、山梨酸、糖精钠、甜蜜素的同时测定.     

高效液相色谱法同时测定复合调味料中2种甜味剂和3种防腐剂

目的建立高效液相色谱法(high performance liquid chromatography,HPLC)同时测定复合调味料中安赛蜜、苯甲酸、山梨酸、脱氢乙酸和糖精钠5种食品添加剂的分析方法。方法样品经超纯水提取,取离心后的水相清液,过0.22μm滤膜,色谱柱为C_(18)柱,流动相为甲醇-0.02 mol/L乙酸铵,柱温为30℃,流速为1.0 mL/min,紫外检测器在230 nm检测,高效液相色谱仪分析。结果本方法5种组分在0.5～50μg/mL范围内具有良好的线性关系,相关系数大于0.99995,加标回收率为91.6%～110.5%,相对标准偏差为0.1%～4.0%。检出限在0.0005～0.0018 g/kg范围,定量限在0.0015～0.0059 g/kg范围。结论该方法操作简单,结果准确,适合复合调味料中安赛蜜、苯甲酸、山梨酸、脱氢乙酸和糖精钠的同时检测。     

高效液相色谱法测定大蒜肠溶片中蒜氨酸的含量

目的:测定大蒜肠溶片中蒜氨酸的含量.方法:采用Zorbax C18色谱柱(250mm×4.6mm, 5μm),柱温25℃,流动相为甲醇:水(30:70),流速0.5ml/min,检测波长为214nm.结果:蒜氨酸浓度在0.0122～0.61mg/ml范围内线性关系良好,平均回收率为97.2%.结论:所建方法简便快速,准确可靠,可用于大蒜肠溶片的含量测定.     

HPLC法同时测定月饼中9种抗氧化剂的研究方法

建立同时对月饼中的叔丁基对羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、叔丁基对苯二酚(TBHQ)、没食子酸丙酯(PG)、2,4,5-三羟基苯丁酮(THBP)、去甲二氢愈创木酸(NDGA)、2,6-二叔丁基-4-羟甲基苯酚(Ionox-100)、没食子酸十二酯(DG)、没食子酸辛酯(OG)9种抗氧化剂进行高效液相色谱(HPLC)测定的研究方法。方法:采用石油醚提取样品中的油脂,乙腈提取目标化合物,用高效液相色谱法测定,以乙腈-1.5%乙酸水为流动相,梯度洗脱,二极管阵列检测器(PAD)定性定量测定月饼中9种抗氧化剂(BHA、BHT、TBHQ、PG、THBP、NDGA、Ionox-100、DG、OG)。结果:在添加浓度1.0～50.0μg/mL范围内,9种抗氧化剂的平均回收率在97.44%～100.01%之间,相对标准偏差(RSD)为0.26%～1.31%。结论:本方法操作简单,可操作性强,有良好的稳定性和重现性,具有广泛推广的意义。     

Automated determination of total polyphenols in apple juice

An automated method of total polyphenols analysis in apple juice using the Folin-Ciocalteu reagent is presented. Chlorogenic acid was selected as the standard since a similar kinetic behaviour, standard-sample, was observed. A straightforward method with good reproducibility (CV <1%), sampling frequency (48 h^-1) and correlation with the traditional batch method (r=0.9924) is proposed.

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Automatische Bestimmung aller Polyphenole in Apfelsaft

Zusammenfassung Es wurde eine automatische Methode zur Erfassung der gesamten Polyphenole in Apfelsaft mittels Folin-Ciocalteu-Reagens angewandt. Chlorogensäure wurde als Standard gewählt, da mit ihr ein ähnliches kinetisches Verhalten in der Standardprobe beobachtet wurde. Es wird eine unkomplizierte Methode mit guter Reproduzierbarkeit (Probenfrequenz C.V. <1%), Probenfrequenz (48 pro h) und gutem Verhältnis zur traditionellen schrittweisen Methode vorgeschlagen.

     

Validation of a HPLC method for simultaneous determination of five sunscreens in lotion preparation

The aim of this research was to develop and validate a high-performance liquid chromatographic (HPLC) method for simultaneous determination of five sunscreens, namely benzophenone-3 (B-3), butyl methoxydibenzoylmethane (BM), octyl methoxycinnamate (OM), octyl salicylate (OS) and homosalate (HS). The separation and quantitative determination was made by HPLC at 40 +/-1 degrees C with a gradient elution from 10% to 100% mobile phase B in mobile phase A. The gradient liquid chromatographic system constituted of mobile phase A [acetonitrile : water (10 : 90 v/v)] and mobile phase B [acetonitrile : water (90 : 10 v/v)], at a flow rate of 1.0 mL min(-1) and ultraviolet detection at 310 nm. The separation was obtained with two Waters reversed phase columns: Novapack C-18 and Symmetry((R)) C-18 connected in series. All sunscreens were efficiently separated within 17 min. The coefficient of correlation and average recovery for B-3, BM, OM, OS and HS were 0.9798 and 98.5%, 0.9672 and 98.8%, 0.9922 and 99.1%, 0.9961 and 98.9% and 0.9909 and 99.4% respectively. The relative standard deviations obtained were between 1.07% and 2.44%. The excipients did not interfere in the analysis. The results showed that the proposed method could be used for rapid and simultaneous determination of B-3, BM, OM, OS and HS in sunscreen lotions with precision, accuracy and specificity.     

苹果渣中多酚物质的福林法测定

以没食子酸为标准品研究了福林法测定苹果渣中多酚物质含量的适宜条件。结果表明,当福林试剂与10%Na2CO3体积之比1∶1,反应温度25℃,反应时间120min时,多酚含量在5～30μg范围内与吸光值呈良好的线性关系。测定方法的平均回收率为106.5%,RSD为0.49%,有较好的准确度和精密度。     

Validation of HPLC method for the simultaneous and quantitative determination of 12 UV-filters in cosmetics

The aim of the study was the validation of a high-performance liquid chromatography (HPLC) method for the simultaneous and quantitative determination of twelve commonly used organic UV-filters (phenylbenzimidazole sulfonic acid, benzophenone-3, isoamyl p -methoxycinnamate, diethylamino hydroxybenzoyl hexyl benzoate, octocrylene, ethylhexyl methoxycinnamate, ethylhexyl salicylate, butyl methoxydibenzoylmethane, diethylhexyl butamido triazone, ethylhexyl triazone, methylene bis -benzotriazolyl tetramethylbutylphenol and bis -ethylhexyloxyphenol methoxyphenyl triazine) contained in suncare products. The separation and quantitative determination was performed in <30 min, using a Symmetry Shield® C18 (5 μm) column from Waters and a mobile phase (gradient mode) consisting of ethanol and acidified water. UV measurements were carried out at multi-wavelengths, according to the absorption of the analytes.     

Validation of a HPLC method for simultaneous determination of main organic acids in fruits and juices

A liquid chromatographic method for fast and simultaneous determination of tartaric, malic, ascorbic and citric acids was validated for further application to fruits and juices. Moreover, the organic acids content of commercial samples of fruits and juices were evaluated, as well as the ascorbic acid stability during the storage. Determination of organic acids was carried out using a liquid chromatograph coupled to a diode array detector, with reversed phase (C₁₈ column) and isocratic elution with 0.01 mol L⁻¹ KH₂PO₄ (pH = 2.60) mobile phase. The validation parameters showed efficiency, adequate linearity, relative standard deviation values between 0.4% and 2.3% (n = 10) for repeatability and from 1.2% to 5.0% (n = 18) for reproducibility, limits of detection (LD) were between 0.03 and 3.31 μg mL⁻¹ and quantification (LQ) were between 0.10 and 11.03 μg mL⁻¹, recovery rates were between 82% and 110%, for two levels. In addition, the method is fast (10 min) and generates low and non-toxic residues. The values found for vitamin C were about 10 times above the values declared at the package. Ready to drink juices have a composition similar to the fruit, concerning to organic acids, except for the powder juice, in which only ascorbic and citric acids were found, for all tastes. After opening the package, a decrease of 14.0% and 27.0% in ascorbic acid content was observed for orange powder and ready to drink juices, respectively.     

Simultaneous determination of nine kinds of preservatives in foods by HPLC

A simple and rapid HPLC method was developed for the simultaneous determination of nine kinds of preservatives, benzoic acid (BA), sorbic acid (SOA), dehydroacetic acid (DHA), methyl p-hydroxybenzoate (PHBA-Me), ethyl p-hydroxybenzoate (PHBA-Et), isopropyl p-hydroxybenzoate (PHBA-isoPu), propyl p-hydroxybenzoate (PHBA-Pu), isobutyl p-hydroxybenzoate (PHBA-isoBu) and butyl p-hydroxybenzoate (PHBA-Bu), in foods. For solid foods, the preservatives were extracted with methanol. After addition of 5 mmol/L citrate buffer to the extract, the extract solution was cleaned up on an Oasis HLB cartridge. The cartridge was washed with 5 mmol/L citrate buffer and methanol-5 mmol/L citrate buffer (4:6). Then, nine kinds of preservatives were eluted with methanol. The eluent was used for BA, SOA and DHA determination by HPLC. Furthermore, a part of the eluent was cleaned up on a Bond Elut PSA cartridge for p-hydroxybenzoate esters determination by HPLC. Liquid foods were cleaned up after addition of 5 mmol/L citrate buffer without the extraction process, and the subsequent procedure was the same as for solid foods. The recoveries of p-hydroxybenzoate esters from ten kinds of foods fortified at levels of 0.01 and 0.10 g/kg each were 91.5 to 107.4%, and those of BA, SOA and DHA were 76.4 to 104.8%. The quantitation limits of the preservatives in foods were 0.005 g/kg. (Received March 20, 2006)     

HPLC测定采后莲雾果实中可溶性糖含量及在贮藏期的变化

建立高效液相色谱法测定台湾"黑珍珠"莲雾果实中的果糖、蔗糖和葡萄糖等可溶性糖含量的方法,并测定采后贮期莲雾果实中可溶性糖含量的变化。色谱条件:采用Waters Carbohydrate柱(4.0μm,4.6mm×250mm),流动相为乙腈/水=90/10(V/V),流速1.5mL/min,柱温45℃。结果表明:利用该法进行色谱分析,各组分能达到较好的分离,在0.625～20mg/mL的糖质量浓度范围内呈现良好的线性关系,相关系数在0.999 8(n=6)以上,3种糖的加标回收率为99.05%～106.39%;精密度试验表明,各组分峰面积RSD为2.55%～3.98%(n=6)。该方法具有较高的灵敏度与精密度,可用于测定采后莲雾果实中的可溶性糖含量及贮藏期间可溶性糖的变化。     

DAD-HPLC法同时测定姜中黄酮类物质

姜具有丰富的营养价值和药用保健功效,也是重要的调味料,具有很大的开发前景。应用二极管阵列高效液相色谱法对姜中黄酮类物质进行了分析,色谱条件为:以HYPERSIR C18BDS为固定相,流动相A甲醇,流动相B 0.1%甲酸水为流动相,采用梯度洗脱,流速0.8m L/min,柱温为30℃,检测波长270nm和370nm。在0¹25mg/L范围内八种黄酮类物质在线性范围内均具有良好的线性关系。结果表明,DAO-HPLC法简便,灵敏,重现性好,可有效的用于姜及姜制品中黄酮类物质含量的测定。      

Analysis of polyphenols in apple products

 Polyphenols of low molecular mass in apple samples were extracted by a C₁₈ solid-phase column, and analysed by HPLC. This extraction method had, in general, a greater extraction ability compared with liquid–liquid extraction using the ethyl acetate method. Received: 11 March 1996