高效液相色谱法测定食物中的类胡萝卜素

综述了用于食物中的类胡萝卜素、类胡萝卜素酯测定的高效液相色谱方法,介绍了样品提取处理方法、色谱分离条件及检测方法。引用文献85篇。     

Determination of Iodide and Thiocyanate in Seawater by Liquid Chromatography with Poly(ethylene glycol) Stationary Phase

Novel, simple, rapid, highly sensitive, and direct determination of iodide and thiocyanate ions in seawater has been performed by liquid chromatography (LC) with UV detection at 220 nm. The separation was achieved on a C₃₀ column of conventional size (150 mm × 4.6 mm i.d.) modified with poly(ethylene glycol); an aqueous solution of 300 mM sodium sulfate and 50 mM sodium chloride was used as mobile phase. Detection limits (S/N=3) obtained by injecting a 20-L sample were 0.5 and 6 ng mL^–1 for iodide and thiocyanate, respectively. The method was successfully used for rapid and direct determination of iodide and thiocyanate in seawater samples, collected from the coasts of Japan, without any extra pretreatment.Dedicated to Professor K. Jinno on the occasion of his 60^th birthday     

Simultaneous Determination of Pioglitazone and Glimepiride by High-Performance Liquid Chromatography

A rapid and accurate HPLC method has been developed for simultaneous determination of pioglitazone and glimepiride. Chromatographic separation of the two pharmaceuticals was performed on a Cosmosil C₁₈ column (150 mm × 4.6 mm, 5 m) with a 45:35:20 (v/v) mixture of 0.01 m triammonium citrate (pH adjusted to 6.95 with orthophosphoric acid), acetonitrile, and methanol as mobile phase, at a flow rate of 1.0 mL min^–1, and detection at 228 nm. Separation was complete in less than 10 min. The method was validated for linearity, accuracy, precision, limit of quantitation, and robustness [1, 2]. Linearity, accuracy, and precision were found to be acceptable over the ranges 2.50–30.00 g mL^–1 for pioglitazone and 0.10–10.00 g mL^–1 for glimepiride.     

高效液相色谱法测定藻类中的类胡萝卜素和叶绿素

提出了用高效液相色谱法测定藻类中类胡萝卜素和叶绿素的方法。采用丙国等有机溶剂提取藻类中的类胡萝卜素和叶绿素,然后在反相C18柱上进行分离。流动相选用二氯甲烷／乙腈／甲醇／水（22.5:9.5:67.5:0.5）,流速为1.0mL／min。用光度检测器检测报长为450um。叶黄素、α-胡萝卜素、β-胡萝卜素、叶绿素a和叶绿素b的平均回收串分别为99.1％,98.5％,99.4％,100.6％和99.9％,相对标准偏差分别为2.4％,5.6％,6.0％,4.1％和4.0％。     

Simultaneous Determination of Trimethoprim, Sulfadiazine, Florfenicol and Oxolinic Acid in Surface Water by Liquid Chromatography Tandem Mass Spectrometry

A liquid chromatographic/tandem mass spectrometric method using atmospheric pressure chemical ionisation (LC-APCI-MS-MS) was developed for simultaneous determination of trimethoprim, sulfadiazine, florfenicol and oxolinic acid in surface water. The compounds were extracted by solid phase extraction on a polymeric sorbent. Two transition products were monitored for each compound. The detection capabilities related to the transition products of lowest abundance were 1 ng L^–1 for trimethoprim, sulfadiazine and florfenicol and 2 ng L^–1 for oxolinic acid. The mean recoveries were 84%, 83%, 96% and 78% at a level of 10 ng L^–1. The relative repeatability standard deviations were less than 11% at a level of 10 ng L^–1.     

A Simple Liquid Chromatography Method for the Determination of Captopril in Urine

A simple and specific method for the determination of total captopril in human urine was developed. 2-Chloro-1-methylquinolinium tetrafluoroborate was used as a thiol precolumn derivatizing reagent after conversion of a disulfide forms to free captopril with tris(2-carboxyethyl)phosphine hydrochloride. The 2-S-quinolinium derivative of captopril was separated on a Zorbax SB C-18 column using reversed-phase ion-paring chromatography and monitored by spectrophotometric detector at 355 nm. The calibration curve for the derivatized captopril showed linearity in the range 0.1–200 μmol L⁻¹ of urine with a regression coefficient corresponding to 0.9999. The detection and quantitation limits were 0.05 and 0.1 μmol L⁻¹, respectively. The intra-day imprecision was from 0.01 to 10.58%. This method can be used for routine clinical monitoring of the thiol-drug. Omission of the reduction step gives result for concentration of the reduced form of captopril.     

Determination of the Enantiomers of Tamsulosin Hydrochloride and its Synthetic Intermediates by Chiral Liquid Chromatography

A chiral liquid chromatographic method is described for the determination of the enantiomers of tamsulosin hydrochloride and its synthetic intermediates. Enantioseparation was achieved on a Chiralcel OD-R column (250 mm × 4.6 mm, 10 m) using a mobile phase consisting of a mixture of 0.5 mol L^–1 sodium perchlorate and acetonitrile (80:20, v/v, pH 4.0). The flow rate was 0.4 mL min^–1 and detection was at 223 nm. Excellent enantiomer separations were achieved for tamsulosin hydrochloride and its synthetic intermediates. No other methods are available for the separation of these enantiomers. The method developed in this study has been successfully applied for purity control.     

Determination of Pyrethroid Insecticide Deltamethrin by Micellar Liquid Chromatography with Spectrophotometric Detection

A simple micellar liquid chromatographic technique for deltamethrin determination was developed and validated. The method provided to be suitable for deltamethrin determination in pediculicide shampoo. Kromasil C18 column (150 mm×4.6 mm, 5 μm) and mobile phase −0.12 M sodium dodecyl sulfate with 9% (v/v) 1-butanol were used for deltamethrin separation. Detection wavelength was 265 nm. The retention time was about 15 min. Different validation parameters were evaluated. The specificity of the method was demonstrated. Linearity was established in the range 10–40 μg L⁻¹. The limits of detection and quantitation were 1.06 and 3.22 μg mL⁻¹, respectively. The method showed excellent accuracy (100.6%) and precision (repeatability) gave a relative standard deviation of less than 1%. The influence of the various method parameters (robustness study) was also studied.     

非水反相液相色谱法测定人血清的类胡萝卜素

采用非水反相－高效液相色谱法（ＮＡＲＰ－ＨＰＬＣ）测定了正常人和胃肠道癌症病人血清的β－胡萝卜素。结果表明,采用外标法定量,回收率为９５％以上,相对标准偏差（ＲＳＤ）最大值为２．２％,分析时间约为２０ｍｉｎ。     

Determination of Polyvinyl Alcohol Using Gel Filtration Liquid Chromatography

Gel filtration chromatography using a TSKgel G2000 SW column coupled with differential refractive index detection was used to analyse five grades of polyvinyl alcohol. Limits of detection and quantification for the assay were 0.14 mg mL^–1, 0.47 mg mL^–1 respectively. The inter and intra-day co-efficient of variance were both <7%. There was a significant difference (p<0.05, n=5) between the calibration curves across the five grades of PVA due to a refractive index range of 13.0790 –1.3181 (n=3). The assay accuracy was 98.99% ± 8.97% (n=5) and 90.60% ± 7.87% (n=5) of a spiked PVA sample was recovered from a commercial formulation.     

水样中农药残留的液相色谱检测

综述了近十五年来液相色谱分析方法在环境水中农药残留分析中的应用,对各种常用的在线和离线样品预浓缩技术、检测器以及液相色谱与质谱等仪器的联用进行了讨论,并对液相色谱在农药残留分析中的应用前景进行了评价。     

反相高效液相色谱法同时测定保健品中的四种类胡萝卜素

建立了不同剂型保健品中类胡萝卜素的提取方法和同时测定保健品中4种类胡萝卜素含量的高效液相色谱分析方法。采用DiamonsilTM C18色谱柱(250 mm×4.6 mm i.d.,5 μm),以乙腈和乙酸乙酯为流动相进行梯度洗脱,洗脱程序：先以100%乙腈洗脱15 min,然后乙酸乙酯的含量在10 min 内从0增加到100%,再以100%乙腈洗脱5 min;流速1 mL/min;采用二极管阵列检测器检测,检测波长为450 nm。以外标法定量,番茄红素、叶黄素、玉米黄素、β-胡萝卜素4种组分的线性关系良好,相关系数为0.9994～0.9997,检测限为0.4～0.5g/L。片剂样品、粉状样品、油状样品的加标回收率分别为95.3%～98.7%,93.7%～98.8%,97.1%～99.2%,相对标准偏差（RSD）分别为0.89%～2.0%,0.89%～2.8%,0.42%～1.2%。该法简便、快速、准确,是保健品中多种类胡萝卜素定量测定的可靠方法之一。     

Simultaneous Determination of Aromatic Amines by Liquid Chromatography Coupled with Carbon Nanotubes/Poly (3-methylthiophene) Modified Dual-Electrode

Liquid chromatography with amperometric detection (LC-AD) is developed and applied to simultaneously determine five aromatic amines. In the LC-AD, a new carbon nanotubes/poly(3-methylthiophene) modified dual-electrode is fabricated and then used as the working electrode. It is found that this chemically modified electrode (CME) exhibits efficiently electrocatalytic oxidation for aromatic amines with relatively high sensitivity, stability and long-life. Thus, lower detection in LC-AD can be achieved, which are 4.0 × 10^–8 mol L^–1 for aniline, 1.6 ×10^–7 mol L^–1 for 4-nitroaniline, 1.0 × 10^–7 mol L^–1 for 4-chloroaniline, 1.5 × 10^–7 mol L^–1 for 1-naphthylamine, 1.7 × 10^–7 mol L^–1 for 2-bromoaniline. The recoveries of the five analytes are also determined, which range between 0.95 and 1.05 for drinking water, 0.86 and 1.10 for the LiWa River water.     

非水反相高效液相色谱法分离测定枸杞子中的类胡萝卜素

采用非水反相高效液相色谱法在ＯＤＳ柱上比较了不同流动相系统对枸杞子中类胡萝卜素的分离效果,探索了枸杞子中类胡萝卜素的最佳分离条件。     

Isocratic Separation of Some Food Additives by Reversed Phase Liquid Chromatography

In recent years, concern about food safety has been growing. The use of food additives in different countries is limited by specific regulations. Therefore, analytical methods that simultaneously determine artificial sweeteners and preservatives are advantageous. High performance liquid chromatography has been the most popular choice for the determination of food additives. In this study, reversed-phase liquid chromatography was developed for the separation of α-aspartame, sodium saccharin, acesulfame-K, vanillin, sorbic acid and benzoic acid. The effects of the proportion of the organic modifier on the chromatographic separation were investigated in order to separate these additives. The results showed that optimum chromatographic separation for these compounds takes place when the acetonitrile content in the mobile phase was 15% containing ammonium acetate buffer (0.005 M). It was concluded that the best separation was obtained with YMC-ODS pack column by using this mobile phase at pH 4.0. All additives were separated within 40 min. The RP-HPLC-UV method was validated in terms of LOD/LOQ, linearity, recovery and repeatability. This method was used for the determination of α-aspartame, acesulfame-K and benzoic acid in cola and instant powder drinks.     

Off-line Coupling of Isotachophoresis and High Performance Liquid Chromatography for Determination of Flavonoids in Plant Extract

Summary The use of isotachophoretic sample pretreatment coupled with high performance liquid chromatography for the analysis of some flavonoids occurring in plant extracts of Hypericum perforatum and Crataegus sp. is described. The samples were extracted with methanol by means of sonication in low temperature. The optimal leading electrolyte was used 10 mM Cl^– as a leading ion in a buffer system at apparent pH^*=7.2 (adjusted by TRIS) and terminating electrolyte was 50 mM boric acid at apparent pH^*=8.2 (adjusted by barium hydroxide). The ITP electrolytes contained 20% (v/v) of methanol. To improve the sample pre-treatment, a pair of discrete ITP spacers defining the trapped constituents was used. Major components presented in the extracts were separated on a Discovery C18 and Discovery RP Amid C16 columns with a gradient mobile phase consisting of methanol, acetonitrile and diluted ortho-phosphoric acid. The quantification was performed by using external standards. The recoveries of the coupled ITP-HPLC analytical procedure were in the range of 91.2–95.6%.     

Method Development for the Determination of Seven Organic Acids in Wines by Reversed-Phase High Performance Liquid Chromatography

A simple high performance liquid chromatographic method is described for the determination of seven organic acids usually found in wines. The acids were eluted in the isocratic mode, in less than 12 min, on a reversed-phase ODS-2 (250 × 4 mm I.D.), 5 m, column with 0.02 M potassium dihydrogen phosphate (pH 2.88), to which was added a small amount of methanol (2%) as organic modifier, and were detected by ultraviolet absorbance at 230 nm. Galacturonic, tartaric, malic (both enantiomers), lactic, acetic, citric and succinic acids were determined, using xanthine as a chromatographic internal standard. The method was applied to white and red wines of Greek origin, after sample clean-up with polyvinylpyrrolidone, followed by passage through SAX cartridges and yielded recoveries from 78.0 to 106.8%. The limits of detection ranged between 0.001–0.05 g.L^–1 and the linear ranges between 0.003–2.0 g.L^–1.     

高效液相色谱法测定萨拉沙星

采用高效液相色谱法测定了萨拉沙星。色谱柱为μ－BondapakTMC18柱（3．9mm×300mm）,流动相为V（乙腈）：V（甲醇）：V（2mmol／L磷酸,用三乙胺调pH3．5）＝30：5：65,用二极管阵列检测器检测,检测波长278nm,得到了满意的分离效果。