高效液相色谱法测定化妆品中依克多因的含量

建立高效液相色谱法测定化妆品中依克多因的分析方法,采用Agilent Poroshell 120 EC-C₁₈色谱柱（100 mm×3.0 mm,2.7μm）分离,以甲醇和p H为3.0的40 mmol/L磷酸二氢钠-10 mmol/L 1-庚烷磺酸钠缓冲溶液梯度洗脱,流速0.8 m L/min,柱温30℃,检测波长210 nm。采用外标法定量测定化妆品中的依克多因含量。结果表明,依克多因在5～800 mg/L的质量浓度范围内呈现良好线性关系,相关系数为0.999 8,方法的检出限和定量限分别为0.3和1.0 mg/L。该方法具有分离效率高、分析时间短、节省溶剂等优点,解决了依克多因在C₁₈色谱柱上保留弱的问题。     

Biogenic amines assessment during different stages of the canning process of skipjack tuna (Katsuwonus pelamis)

The present research focused on the biogenic amines (BAs) formation in skipjack tuna (Katsuwonus pelamis) throughout the whole canning process. In agreement with its wide employment on this species, on‐board brine immersion freezing (BIF) was tested as post‐mortem processing. The study included fish samples corresponding to different stages of the canning process such as frozen, thawed, cooked and canned; after cooking, two kinds of tuna muscles were considered, that is, whole fillets (main product) and grated muscle (off‐product arising from small pieces). For the BAs (tryptamine, putrescine, cadaverine, histamine, spermidine and spermine) assessment, an HPLC‐DAD method was developed and validated in skipjack tuna samples, in agreement with different parameters such as suitability, linearity, limits of detection and quantification, precision, accuracy and robustness. Tuna submitted on‐board to BIF procedure provided low levels of spermine and spermidine (up to 27.6 mg kg^?1), while contents on the remaining BAs maintained below the limit of detection. Throughout the different stages of the canning process, skipjack tuna showed a low formation of most BAs; interestingly, histamine content was found below 10.6 mg kg^?1 level. The highest values were obtained for spermidine, these related to cooked grated tuna (from 22.6 to 66.7 mg kg^?1) and canned grated tuna (from 70.6 to 104.4 mg kg^?1). Values for pH assessment in all kinds of tuna samples corroborated the results obtained for BAs determination. BIF procedure proved to be an amenable post‐mortem processing to guarantee the quality of canned skipjack tuna.     

Detection and analysis of triterpenic compounds in apple extracts

A new technique for the rapid detection and analysis of triterpenic compounds in apple extracts using HPLC was developed and validated. The main advantage of this technique is the short duration of the analysis – this makes this technique superior to others currently applied for the routine HPLC analysis of triterpenic compounds. The developed, optimized, and validated technique was used for the evaluation of triterpenic compounds in samples of different cultivars of apples, their peels, and flesh. In total, four triterpenic compounds were isolated and identified. Ursolic acid was the dominant compound in all the tested apple samples. The highest amounts of triterpenic compounds were detected in the peels of the ‘Lodel’ apple cultivar, and thus apples of this cultivar may be potentially useful for the isolation of individual compounds and the production of functional food and dietary supplements.     

超声辅助离子液体/阴离子表面活性剂双水相萃取虎杖中的虎杖苷和白藜芦醇

将超声辅助离子液体/阴离子表面活性剂双水相萃取和高效液相色谱法相结合,建立一种简单、绿色、高效的分析方法用于检测虎杖中的虎杖苷和白藜芦醇。本研究以水溶性离子液体为萃取剂,以阴离子表面活性剂为成相盐,在超声的辅助作用下,目标分析物被萃取于离子液体中。实验结果表明,最佳提取条件为:以400μL 1-丁基-3-甲基咪唑四氟硼酸盐为萃取剂,0.16 g十二烷基苯磺酸钠为成相盐,样品溶液pH 7.0,超声时间20 min,超声功率160 W。各化合物在线性范围内都具有良好的线性关系(r0.9995),日内和日间精密度分别低于3.27%和6.31%,检出限和定量限分别为2.8~12.3和9.4~41.1 ng/mL,样品加标回收率在86.88~94.13%之间。本研究采用离子液体代替传统的有机溶剂作为萃取剂,集提取、分离和纯化于一体,具有操作简单、溶剂用量少、提取时间短等优点,可广泛应用于中药活性成分的提取与分析。     

GC和HPLC分析金银花多糖的单糖组成方法比较

目的:GC法和HPLC法分析金银花多糖的单糖组成,并对两种方法进行比较。方法:金银花多糖经2.0 mol·L-1的三氟乙酸水解后,用糖腈乙酸酯衍生化-GC法和1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生化-HPLC法分别测定其单糖组成及其比例。结果:GC法检测出金银花多糖由鼠李糖(L-Rha)、阿拉伯糖(D-Ara)、甘露糖(D-Man)、木糖(D-Xyl)、葡萄糖(D-Glc)、半乳糖(D-Gal)组成;HPLC法检测到金银花多糖中含有甘露糖(D-Man)、鼠李糖(L-Rha)、葡萄糖醛酸(D-GlcA)、葡萄糖(D-Glc)、半乳糖(D-Gal)、阿拉伯糖(D-Ara)和木糖(D-Xyl),其中半乳糖(D-Gal)与阿拉伯糖(D-Ara)的色谱峰重叠。结论:两种方法均能检测出中性糖,HPLC法不仅能测中性糖,还能检测出葡萄糖醛酸,对金银花多糖的单糖组成分析GC与HPLC联合使用较为合适。     

高效液相色谱-串联质谱联用法与高效液相色谱法同步测定白玉菇麦角固醇和VD_2方法比较

建立高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLCMS/MS)联用法与HPLC法同步检测白玉菇样品中麦角固醇和VD2含量方法,经方法学评价确定两种检测方法的线性范围、灵敏度与精确性。通过对经醇碱皂化回流法提取样品中麦角固醇和VD2的分析验证,阐述两种检测方法的差异性,为白玉菇有效生物活性成分与相关产品的质量检测和对白玉菇中麦角固醇与VD2之间转化关系的研究提供技术支持。HPLC-MS/MS法中,采用色谱分离柱Agilent SB-C8 Rapid Res柱(2.1 mm×50 mm,3.5μm)及在优化的色谱条件下,麦角固醇与VD2之间色谱峰保留时间分别为4.303 min和4.22 min。电喷雾离子源正离子模式下采用多反应选择离子监测模式,分别选择m/z 379.3/125.3与m/z 397.3/125.3离子对麦角固醇与VD2进行定量,结果表明麦角固醇在0.15～6 mg/L、VD2在0.01～1 mg/L范围内与峰面积线性关系良好,平均加标回收率分别为93.51%、90.56%,日内和日间相对标准偏差均小于7%。HPLC法采用COSMOSIL Column 5C18-MS-II(4.6 mm×250 mm,5μm)柱分离体系,麦角固醇和VD2色谱峰保留时间分别为12.891 min和9.919 min,方法学评价结果显示,麦角固醇在15～750 mg/L、VD2在0.5～50 mg/L范围内与峰面积线性关系良好,两者的平均回收率分别为98.51%、94.05%,日内和日间相对标准偏差均小于1%。采集的样品采用HPLC-MS/MS联用法和HPLC法分别检测实验结果有一定的差异,与HPLC法相比,HPLC-MS/MS联用法具有快速检测时间短、检出限低、更灵敏的优势。     

柱前衍生化HPLC法分析枸杞多糖中单糖组成

利用1-苯基-3-甲基-5-吡唑啉酮柱前衍生化高效液相色谱(high performance liquid chromatography,HPLC)法,建立6种常见单糖的色谱分离条件,并用于10种不同产地的自制枸杞多糖的单糖组成分析和8种市售枸杞多糖的分析鉴定。该HPLC方法简便、灵敏度高、重复性好,可用于枸杞多糖的组分分析和质量控制。对自制枸杞多糖的单糖组成分析结果表明,自制枸杞多糖由甘露糖、鼠李糖、半乳糖醛酸、葡萄糖、半乳糖及阿拉伯糖6种单糖组成,平均物质的量比为1.00∶1.38∶0.63∶92.37∶1.18∶3.55。对市售枸杞多糖的分析鉴定结果表明,其中6种枸杞多糖的含量在正常范围内,另外2种多糖含量高于均值,其中葡萄糖相对物质的量比为自制枸杞多糖的2~3倍。     

脱苦过程中苦杏仁苷含量的变化及其与苦味的关系

借助奎宁标准品进行苦味鉴评,探究苦杏仁中苦杏仁苷含量与苦味的关系。以脱皮苦杏仁为研究对象,进行水浴脱苦[脱苦温度70℃、料液比1:12(g/mL)、脱苦时间6h],每30min取样一次,对各样品进行感官评定,并采用高效液相色谱法(HPLC)测定样品中的苦杏仁苷含量。结果表明:苦杏仁中苦杏仁苷含量与苦味呈正相关关系,70℃水浴脱苦5h后,苦杏仁中苦杏仁苷含量低至0.91mg/g·干基,苦杏仁苦味等级降为Ⅰ级,品尝时已不苦。苦杏仁中苦杏仁苷含量与苦味密切相关,运用HPLC测定苦杏仁中苦杏仁苷的残留量即可准确判断其脱苦程度。     

液态发酵红曲黄色素粗提物色素组分的分离纯化与鉴定

采用高效液相色谱、质谱和核磁共振分析,对液态发酵红曲黄色素粗提物色素组分进行分离纯化和分子结构鉴定,确定其化学结构式。结果表明,红曲黄色素有2种主要色素成分,组分A和组分B,两者在分析型液相色谱上分离度达到2.51。进一步将分析型液相分离条件在制备型液相上进行放大并调整,收集得到组分A和组分B,纯度分别为98.95%和99.02%,达到标准品的纯度。通过质谱分析结合一维及二维核磁共振,确定组分A的相对分子质量为358,为红曲素(C21H26O5),组分B的相对分子质量为332,为Monaphilone B(C20H28O4),A和B的显色性能来自于其分子结构中的α,β-不饱和酮结构。