Flow injection on-line dialysis coupled to high performance liquid chromatography for the determination of some organic acids in wine

A combined system of flow injection on-line dialysis sample pretreatment and high performance liquid chromatographic separation/detection (FID-HPLC) was developed for simultaneous determination of six organic acids (tartaric, malic, lactic, acetic, citric and succinic acids). A sample or mixed standard solution (400 μL) was injected into a donor stream (water) of FID system and was pushed further through a dialysis cell, while an acceptor solution (water) was held in the opposite side of the dialysis membrane. The dialysate containing organic acids in the acceptor solution was then flowed to an injection loop of the HPLC valve, where it was further injected into the HPLC system and analysed under normal HPLC conditions, using a reversed-phase (C₁₈) analytical column and UV detection (210 nm). The order of elution was tartaric, malic, lactic, acetic, citric and succinic acids with the analysis time of 8 min. The FID system could be operated in parallel with HPLC separation, providing sample throughput of 7.5 h⁻¹. Dialysis efficiencies of six organic acids were in range of 4.6-9.5%. Calibration graphs for all the mentioned organic acids were linear over the range of 250-7500 mg L⁻¹. Precisions for all the organic acids were within 5.4%. The proposed system was successfully applied for analysis of some Thai wines. By spiking wine samples with mixed acid standard solutions, the percentage recoveries in range of 84-104 were found. This system has advantages of fast and high degrees of automation for dialysis sample pretreatment, on-line sample separation and dilution, good clean-up for prolongation of life-time of the HPLC column and low consumption of chemicals and materials.     

高效液相色谱法同时测定食品中的5种添加剂

采用高效液相色谱法测定了食品中山梨酸、苯甲酸、糖精钠、乙酰磺胺酸钾和脱氢乙酸等5种食品添加剂.结果表明:高效液相色谱法能够满足食品中5种食品添加剂同时测定的要求;在0～200 mg/L的线性范围内.相关系数r大于0.999 2,对5种食品添加剂的最低检出限分别为0.15、0.25、0.45、0.17、0.23 mg/k...     

Simultaneous determination of 20 food additives by high performance liquid chromatography with photo-diode array detector

An efficient and accurate analytical method was developed for the simultaneous determination of 20 synthetic food additives, including three sweeteners,seven food colorants,nine synthetic preservatives and caffeine,by high performance liquid chromatography (HPLC) with photodiode array detector(PDA).This method permits the detection of food additives at very low concentrations(0.005-0.150μg/mL).The applicability was verified by the determination of food additives present in various foodstuffs.     

高效液相色谱法同时测定肉制品中的6种食品添加剂

建立了同时测定肉制品中化学性质差异较大的6种常用食品添加剂的高效液相色谱(HPLC)分析方法。根据6种添加剂(苯甲酸(钠)、山梨酸(钾)、糖精钠、安赛蜜、诱惑红和胭脂红)的化学性质,对HPLC分析条件进行了详细的优化。结果表明:以ZORBAX Eclipse Plus C18柱(150mm×4.6mm,5μm)为分析柱,以甲醇和20mmol/L醋酸铵溶液(pH为6.9)为流动相进行梯度洗脱,在235nm波长下进行检测,可以在18min内完成6种添加剂的同时测定。在高、低两个加标浓度下,样品的回收率为80.7%～94.4%,相对标准偏差(n=3)为2.0%～7.1%。结果表明,该方法快速、准确,能够同时分析测定肉制品中上述6种食品添加剂。     

高效液相色谱法测定保健食品和饮料中的阿斯巴甜

建立了保健食品和饮料中的甜味剂阿斯巴甜的高效液相色谱快速测定方法.固体样品用纯水超声提取;饮料样品超声脱气.取适量提取液或饮料样品,经0.45 μm滤膜过滤后,取20 μL进样色谱柱分析.色谱条件:分离柱为C18柱(250mm×4.6 mm i.d.,10μm),柱温35℃,流动相为V(10 mmol/L KH2PO4,pH 3.50):V(乙腈)=80:20,流速1 mL/min,检测波长210 nm.本法线性范围为0～16 μg,最低检出量为0.0024 μg,回收率为92.3%～102%.相对标准差小于1.6%.本法准确度和精密度均能满足保健食品和饮料中阿斯巴甜测定的要求.     

Emulsification liquid phase microextraction followed by on-line phase separation coupled to high performance liquid chromatography

An emulsification liquid phase microextraction followed by on-line phase separation coupled to high performance liquid chromatography (HPLC) is introduced based on a novel idea for the separation of dispersed organic phase from aqueous phase. In this method, the dispersed organic extraction phase was filtered using an in-line filter and it was separated from the water sample. The new approach is simple and, in addition to improving some limitations of the conventional emulsification liquid phase microextraction, eliminates the need for centrifugation in the phase separation step.     

高效液相色谱法同时测定蜜饯中5种常见食品添加剂

建立同时测定蜜饯中安赛蜜、苯甲酸、山梨酸、糖精钠、脱氢乙酸的反相高效液相色谱法,用于监测蜜饯产品,提高时效性.安赛蜜、苯甲酸、山梨酸、糖精钠、脱氢乙酸分别在1.2～100 μg/mL、0.2～100 μg/mL、1.1～100μg/mL、6.2～140 μg/mL和2.7～100 μg/mL浓度范围内线性良好,相关系数分别为0.9997、0.9999、0.9996、0.9998和0.9993,检出限分别为15、1.2、18、50和20 ng;平均回收率均在95%以上,相对标准偏差均小于2.8%.此法样品处理简便易行,适于同时测定蜜饯中的安赛蜜、苯甲酸、山梨酸、糖精钠、脱氢乙酸.     

高效液相色谱法测定保健食品中的大豆异黄酮

建立了一种测定保健食品中大豆异黄酮的高效液相色谱分析方法,该方法可以使常见的大豆异黄酮6种主要成分大豆甙、黄豆甙、染料木甙、大豆甙元、黄豆黄素、染料木素得以分离和检测。采用乙腈-磷酸水溶液(pH2.8)作流动相,梯度洗脱,Venusil MP-C18色谱柱(150 mm×4.6 mmi.d.,5μm),流速为1.0 mL/min,紫外检测器,检测波长254 nm。结果表明各组分线性关系良好,相关系数R2为0.9991~0.9998,加标回收率在87%~106.9%,相对标准偏差均小于2%。检出限0.25~0.48μg/mL,该方法可同时测定大豆异黄酮的6种成分。     

高效液相色谱法同时测定食品中安赛蜜、糖精、苯甲酸、山梨酸和咖啡因

用KromasilC1 8柱 ,以甲醇 :0 .5g/L柠檬酸铵 (42 5 :5 75 )为流动相 ,在波长 2 1 5nm ,柱温 40℃下测定了食品中的安赛蜜、糖精、苯甲酸、山梨酸和咖啡因。方法RSD 0 .6 2 %～ 1 48% ,回收率 1 0 0 .7%～ 1 0 3 % ,相关系数r>0 .9998;应用于可乐、汽水、果奶等测定。     

固相萃取-高效液相色谱法同时测定食品中4种合成色素

以可代替使用的水溶性合成色素-亮黑BN、固绿FCF、酸性红、酸性黄36为研究对象,建立了高效液相色谱同时测定食品中4种合成色素的方法。样品通过WAX固相萃取柱富集净化,10%氨化甲醇洗脱,采用C18色谱柱分离,以甲醇和10 mmol/L乙酸铵水溶液作为流动相梯度洗脱,外标法定量。通过固相萃取柱净化后,杂质对待测物的干扰明显降低,优化色谱条件下,4种色素在0.10~10.0 mg/L质量浓度范围内,线性良好,相关系数(r)≥0.9995。方法回收率为92.6%~101.8%,相对标准偏差(RSD)≤5.4%,方法检出限为0.01~0.04 mg/kg。该方法灵敏度高,准确可靠,适合食品中亮黑BN、固绿FCF、酸性红、酸性黄36的同时测定。     

反相高效液相色谱法同时测定水样中辛硫磷和氯菊酯

采用AgilentSBC8(5μm,4.6mmi.d.×150mm)色谱柱,以V(乙腈)∶V(水)=70∶30为流动相进行分离,二极管阵列检测器(PDA)在210nm波长处检测,建立了反相高效液相色谱法同时测定辛硫磷和氯菊酯的分析方法。辛硫磷和氯菊酯的线性范围分别为0.1～10μg mL和0.02～10μg mL,检出限分别为0 05和0.01μg mL,实际水样的加标回收率为90.3%和95.3%,相对标准偏差为1.3%和3.2%(n=7)。     

Automated high performance liquid chromatography with on-line reduction of disulfides and chemiluminescence detection for determination of thiols and disulfides in biological fluids

In general, the reduction of disulfide bonds with tris(2-carboxyethyl)phosphine (TCEP) is performed using off-line operation, which is not only time-consuming but also vulnerable to the spontaneous re-oxidation of thiols during sample preparation and subsequent analysis procedures. To the best of our knowledge, there has been not any case on the on-line reduction for biological disulfides coupled with high performance liquid chromatography (HPLC). In this study, these obstacles are overcome by packing Zn(II)-TCEP complexes into a home-made column. The as-synthesized Zn(II)-TCEP complexes enable efficient reduction of disulfide bonds at pH 3.0. This acidic pH value was compatible with that of the mobile phase for HPLC separation of thiols and disulfides. Therefore, using fluorosurfactant-prepared triangular gold nanoparticles as HPLC postcolumn specific chemiluminescence (CL) reagents for thiols, the feasibility of the established on-line reduction column has been confirmed for the direct identification of both thiols and disulfides by incorporating this reduction column into a single chromatographic separation. Detection limits for these analytes range from 8.3 to 25.4 nM and the linear range in a log–log plot can comprise three orders of magnitude. Finally, the utility of this automated on-line reduction of disulfides-HPLC-CL system has been demonstrated for the reliable determination of thiols and disulfides in human urine and plasma samples.     

高效液相色谱手性流动相法拆分酮基布洛芬对映体

以Lichrospher C18为分析柱, 将β-环糊精、2,6-二甲基-β-环糊精、2,3,6-三甲基-β-环糊精分别作为手性流动相添加剂, 系统地研究了R,S-酮基布络芬对映体在HPLC系统中的拆分. 建立了以2,3,6-三甲基-β-环糊精为手性流动相添加剂分离R,S-酮基布络芬对映体方法.     

超声波辅助萃取－高效液相色谱法测定食品中碱性玫瑰精

建立超声波辅助萃取—高效液相色谱法测定含辣椒食品中非法添加剂碱性玫瑰精的方法.样品经均质,辣椒面样品、辣椒油样品、红油豆瓣酱样品分别用乙腈:水=7:3(V/V)溶液、正己烷:50％乙醇=1:2(V/V)溶液、无水乙醇经超声波辅助萃取后,用高效液相色谱仪测定碱性玫瑰精.线性范围0.026～26 μg/mL,相关系数0.9...     

Carrier-mediated liquid phase microextraction coupled with high performance liquid chromatography for determination of illicit drugs in human urine

A new method was developed for the analysis of illicit drugs in human urine by coupling carrier-mediated liquid phase microextraction (LPME) to high performance liquid chromatography (HPLC). By adding an appropriate carrier in organic phase, simultaneous extraction and enrichment of hydrophilic (morphine and ephedrine) and hydrophobic (pethidine) drugs were achieved. Effects of the types of organic solvents and carriers, the carrier concentration in the organic phase, the HCl concentration in the acceptor solution, the stirring rate, and the extraction time on the enrichment factor of analytes were investigated. Under the optimal experimental conditions, high enrichment factors (202-515) were obtained. The linear detection ranges were 0.1-10 mg L⁻¹ for the studied drugs. The limits of detection (LOD) at signal-to-noise ratio of 3 were 0.05 mg L⁻¹ for both morphine and ephedrine, and 0.02 mg L⁻¹ for pethidine. This method was successfully applied to analysis of ephedrine in real urine specimens, revealing that the determination of illicit drugs in urine was feasible.     

固相萃取-高效液相色谱法同时测定水中的对二氯苯与六氯苯

采用国产新型D4020 大孔吸附树脂作固定相,用自制的玻璃富集柱研究了柱长、上样速度、样品溶液的pH、盐度等因素对对二氯苯与六氯苯吸附率的影响,确定了最佳固相萃取条件,建立了固相萃取-高效液相色谱同时测定水中痕量对二氯苯与六氯苯的分析方法;不同加标水平的对二氯苯与六氯苯的回收率为86.4%～93.9%,RSD≤4.2%,检出限分别为0.85和0.10 ng/mL;方法已用于实际水样分析.     

高效液相色谱法同时测定食品接触材料中抗氧化剂和紫外吸收剂的迁移量

采用高效液相色谱技术,建立了食品接触材料中多种抗氧化剂和紫外吸收剂迁移水平的检测方法。该方法测定的23种目标化合物具有较好的线性关系,相关系数（r²）≥ 0.9998,检出限和定量限分别在0.01到0.22 mg/L之间和0.03到0.85 mg/L之间。依据欧盟指令（EU）No. 10/2011,考察了5种食品模拟物30 g/L乙酸、10%（v/v）乙醇、20%（v/v）乙醇、50%（v/v）乙醇和油类模拟物（异辛烷）中抗氧化剂和紫外吸收剂的迁移量。该方法回收率在92.8%~117.7%之间,相对标准偏差在0.95%~9.72%之间。探讨了不同实验条件对抗氧化剂和紫外吸收剂回收率的影响。结果表明,该方法准确、稳定,完全满足欧盟指令（EU）No 10/2011和GB 9685-2008对食品接触材料及制品中抗氧化剂和紫外吸收剂特定迁移量（SML）的限量要求,并利用该方法测定了30批次食品接触材料中抗氧化剂和紫外吸收剂的迁移水平。     

高效液相色谱-气相色谱在线联用同时测定土壤中饱和烃和芳香烃

为加强对土壤中石油烃类污染物的风险管控,生态环境部已将石油烃类列为土壤中的重点监测项目.石油烃源于石油与合成油,是涵盖一定碳数范围的碳氢化合物,主要分为饱和烃和芳香烃两大类.芳香烃通常是高度烷基化的单环、双环与多环芳烃,其对人和动物的毒性较饱和烃大很多,因此,仅仅测定土壤中总石油烃含量难以准确评估其环境毒性.目前环境领...     

离子液体作高效液相色谱流动相添加剂分离测定芳香胺

建立了以离子液体作反相高效液相色谱流动相添加剂分离测定邻苯二胺、苯胺和对甲苯胺3种芳香胺的方法。实验以C18反相色谱柱为分离柱,采用紫外检测方法,考察了检测波长、甲醇含量、咪唑离子液体烷基链长度、离子液体溶液浓度等条件对分离和测定的影响,并与其它分离测定芳香胺的方法进行了比较。优化的色谱条件为:以甲醇/1-丁基-3-甲基咪唑四氟硼酸盐水溶液(3.0mmol/L,乙酸调节pH 3.5)=30/70(V/V)为流动相;检测波长254 nm;流速1.0mL/min;柱温30℃。在此条件下,3种芳香胺达到基线分离,在6.5 min之内分离完全;在1～40 mg/L范围内,线性回归方程的相关系数达到0.99以上;检出限为0.07～0.41 mg/L。将本方法应用于废水的测定,加标回收率在92.3%～96.7%之间,相对标准偏差小于3.5%。     

高效液相色谱法测定胭脂红酸的研究

研究了以反相C18柱,V(甲醇)∶V(乙腈)∶V(pH 2.8 H3PO4)=12∶8∶80混合溶液为流动相,对胭脂红酸进行高效液相色谱分析的方法。胭脂红酸在2.5~40μg/mL范围内的吸光度线性相关系数达0.9998,方法回收率在98.2%~101.1%,相对标准偏差为0.78%~1.2%,已用于样品中胭脂红酸的测定。