乙酰丙酮衍生化高效液相色谱-荧光检测法测定食品中的甲醛

建立基于乙酰丙酮衍生化利用配有荧光检测器高效液相色谱测定食品中甲醛含量的方法。色谱柱为EclipseXDB-C18（250 mm×4.6 mm,5 μm）,流动相为V（乙腈）∶V（水）=20∶80,激发波长为416 nm,发射波长为505 nm,采用外标法定量,甲醛质量浓度在0.001～20.0 mg/L范围内呈良好线性,相关系数为0.999 9。甲醛质量浓度为0.005、0.05、0.5、5.0 mg/L时相对标准偏差分别为4.2%、1.9%、1.4%和0.81%。固体及粉末样品的检出限为0.025 mg/kg,液体样品的检出限为0.025 mg/L。本方法用于干香菇、面粉及啤酒样品中甲醛含量的测定,加标回收率为92.0%～97.7%,相对标准偏差不大于5.6%。结果表明,本方法灵敏度高,方便快捷,结果可靠。     

免疫亲和柱净化-高效液相色谱法检测两种饮料中双酚A含量

建立了免疫亲和柱净化-高效液相色谱荧光检测法(IAC-HPLC-FL)检测豆奶及橙汁饮料中的双酚A含量。采用甲醇提取、离心、磷酸缓冲溶液稀释后,经免疫亲和柱纯化,用1 mL甲醇-水(80:20,体积/体积)洗脱,应用高效液相色谱法检测。以C₁₈柱为分离色谱柱,甲醇-水(60:40,v/v)溶液为流动相洗脱,流速0.4 mL/min,柱温30℃,进样量10 μL,荧光检测器检测,激发波长228 nm,发射波长310 nm。结果表明:在1.0~300.0 ng/mL的浓度范围内,双酚A的浓度与峰面积呈良好的线性关系(相关系数R²=0.9998),检出限定为1 ng/mL。平均回收率为82.5%~104.6%,相对标准差为2.3%~6.4%。分别选取玻璃瓶装和塑料瓶装的豆奶和橙汁饮料进行双酚A含量检测,玻璃瓶装的豆奶和橙汁饮料中双酚A含量均小于检出限1 ng/mL,而某款塑料瓶装的豆奶和橙汁饮料检测出极其微量的双酚A,其双酚A含量分别为1.44、1.57 ng/mL,处于可接受水平。该方法简单快速、灵敏度高、重复性好,能够有效地分离和检测饮料中的双酚A,适用于豆奶和橙汁等饮料中的双酚A的测定。     

HPLC-FL法检测尿液中类雌激素双酚A和烷基酚

目的建立尿液中类雌激素（壬基酚（NP）、辛基酚（OP）和双酚A（BPA））的HPLC-荧光测定方法。方法采用β-葡萄糖酸酐酶、硫酸酯酶水解人尿液中的结合型壬基酚、辛基酚和双酚A,酶解后溶液采用OASIS HLB固相萃取柱浓缩、畜集和净化。Watersx Terra^TM MS C18液相色谱柱分离,甲醇＋水作为流动相梯度洗脱。荧光检测,激发波长：225nm;发射波长：310nm。结果NP、OP和BPA具有良好的线性关系,BPA、NP和OP的检出限分别为3．7、4、9和7．5ng／ml,BPA、NP和OP加标回收率分别为：70．2％-95．7％、73．2％～108、2％和76．3％～109．1％;船D分别为5．61％～8．19％、6．01％～7．98％和6、23％～8．61％。结论该方法测定尿液中类雌激素（BPA、OP和NP）,具有较高的灵敏度和选择性,结果准确可靠、重现性好。     

Simultaneous Determination of Nine Quinolones in Food by Liquid Chromatography with Fluorescence Detection

A confirmatory analytical method for simultaneous determination of nine regulated quinolones (Council Regulation 2377/90/ECC) in six matrices of animal origin is proposed. The sample pretreatment involves double step liquid extraction with acetonitrile and purification by solid-phase extraction on Oasis HLB cartridges. The quinolones were separated by liquid chromatography on C18 Zorbax column with gradient elution program. Aqueous formic acid, methanol, and acetonitrile were used as a mobile phase. A multi-wavelength excitation/emission program was used for sensitive fluorescence detection of quinolones. The proposed sample pretreatment protocol was applied to each of the six studied matrices without any modification. The method was validated according to Commission Decision 2002/657 EC. Residues were quantified down to 15 μg kg^?1 with limits of detection and quantification ranging from 3 to 50 μg kg^?1 and from 7.5 to 100 μg kg^?1, respectively. The recoveries at the maximum residual limits (MRLs) were between 77 and 120 % with RSD values lower than 30 %. For quinolones without established MRL or maximum required performance limit, the accuracy and precision of the method were estimated at concentration levels corresponding to the lowest linear calibration point and recoveries between 70 and 130 % were achieved. Decision limits, detection capability, and linear range in eggs, milk, fish, ovine muscle, chicken muscle, and porcine kidney are also reported.     

多杀菌素的高效液相色谱测定

本文建立了高效液相色谱法测定多杀菌素的定量分析方法,本方法的相对标准偏差为1.3441,变异系数为1.8067%,线性相关系数为0.99959,平均回收率达到99.2429%,最后采用液质联用方法对目标化合物进行验证.     

高效液相色谱法测定纸质食品接触材料中双酚A和双酚S的含量

该文建立一种测定纸质食品接触材料中双酚A和双酚S含量的高效液相色谱(high performance liquid chromatography,HPLC)法.方法分析采用Thermal Ultimate 3000SD液相色谱仪,ZORBAX Eclipse XDB-CN(250 mm×4.6 mm,5μm)反相柱.流...     

高压液相色谱法测定可乐饮料中咖啡因的探讨

<正> 饮料中咖啡因的高压液相色谱法测定,国内目前尚未见报道。本人参考国外有关文献,利用国产仪器和填料,研究了样品不经化学处理,直接进样测定咖啡因的色谱条件和可行性,结果较为满意,平均回收率为100.05％,该法简单快速,灵敏度高,测定一个样品仅需     

高效液相色谱法测定食品中番泻苷A和番泻苷B的含量

建立高效液相色谱法测定食品中番泻苷A和番泻苷B的方法。样品经过0.2%碳酸氢钠溶液超声提取,采用Agilent ZORBAX SB-C₈(4.6 mm×150 mm,5.0 μm)色谱柱分离,以四氢呋喃-水-乙酸为流动相洗脱,DAD检测器,检测波长:340 nm。番泻苷A、番泻苷B在1～100 μg/mL范围线性关系良好,相关系数均大于0.999,检出限(S/N=3)为15 mg/kg,定量限(S/N≥10)为50 mg/kg。以空白样品进行添加回收试验,番泻苷A的回收率为80.88%～96.34%,相对标准偏差(Relative Standard Deviation)为3.07%～7.73%,番泻苷B的回收率为81.32%～102.2%,相对标准偏差(RSD)为2.62%～9.62%。该方法前处理简单、灵敏度高、操作简便、准确性良好。在市售的果冻类食品中,检出阳性样品。     

HPLC法测定乳饮料中纽甜含量的研究

建立快速、准确测定乳饮料中纽甜含量的高效液相色谱检测方法。样品以20%乙腈水溶液为提取液,硫酸锌和亚铁氰化钾为沉淀剂进行前处理,采用ZORBAX SB-C18(250 mm×4.6 mm,5μm)色谱柱,200 nm检测波长,磷酸氢二铵(0.020 mol/L,pH 3.5~4):乙腈=(70∶30)为流动相进行等度洗脱分离。纽甜在0.2μg/m L~50.0μg/m L范围内线性良好,在0.8 mg/kg~5.0 mg/kg加标范围内,回收率为90.1%~96.1%,RSD值为1.7%~2.1%,最低定量限为0.30 mg/kg。     

Determination of Chlorantraniliprole Residues in Grape by High-Performance Liquid Chromatography

An effective analytical method for the residue analysis of a novel insecticide chlorantraniliprole and its dissipation in grape were studied. Chlorantraniliprole residues were extracted from grape samples with ethyl acetate. The extract was cleaned up with QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and determined by high-performance liquid chromatography with photodiode array detector (HPLC-DAD). At fortification levels of 0.06, 0.5, and 1.0 mg kg^?1 in grape, it was shown that recoveries ranged from 95.11 to 102 % with relative standard deviation (RSD) of 6 to 11 %. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.02 and 0.06 mg kg^?1, respectively. The dissipation half-life time of chlorantraniliprole residues in grape was 2.70 days. According to maximum residue limit (MRL), the preharvest interval (PHI) of chlorantraniliprole on grape was 4 days after the treatment. Based on the results of this study and the relevant residue regulation, chlorantraniliprole residue levels will be acceptable when applied to grape in Egypt.     

Sensitive Determination of Decoquinate in Milk by High-Performance Liquid Chromatographic Coupled to Laser-Induced Fluorescence Detection

A new and sensitive method based on high performance liquid chromatography with laser-induced fluorescence detection has been developed for the determination of decoquinate in milk. Laser source was obtained with a He–Cd laser using a continuous excitation wavelength at 325 nm. Decoquinate exhibits moderate fluorescence, but it is increased using Ca(NO₃)₂ in the mobile phase. The chromatographic separation was performed on a Luna C₁₈ 5-mm reversed phase column, which solves the broadening of peaks and peak tailing compared with other columns tested. The mobile phase, delivered at 1 ml min⁻¹, consisted of methanol–calcium nitrate (0.025 M)–acetonitrile (83/13/4 v/v/v). Decoquinate was successfully cleaned up from milk by solid-phase extraction using C₁₈ cartridges. The method was found to be linear between 0.16 and 16.33 ng ml⁻¹. The results of recovery studies were found to be satisfactory; an average recovery rate of 88.7% was obtained. The LOQ of decoquinate in milk was 0.16 ng ml⁻¹. The intraday relative standard deviation (RSD) was 4%, and interday assay gave an RSD of 4.4%.     

超高效液相色谱串联质谱法测定全蛋粉中的双酚A和双酚S

建立超高效液相色谱-串联质谱测定全蛋粉中双酚A和双酚S的检测方法。全蛋粉经水复溶后经乙腈提取,提取液使用分散系固相萃取-基质增强脂质去除产品进行除脂,使用Oasis PRiME HLB小柱进一步净化,使用超高效液相串联质谱测定,负离子多反应监测(MRM)模式测定,内标法定量。结果显示:双酚A在1~50 μg/kg范围内呈线性,相关系数为0.9991,加标回收率为98.8%~105.0%,日内和日间相对标准偏差分别为3.84%~8.58%和5.65%~8.74%,检出限为0.3 μg/kg,定量限为1.0 μg/kg;双酚S在0.4~20 μg/kg范围内呈线性,相关系数为0.9995,加标回收率为98.5%~102.5%,日内和日间相对标准偏差分别为3.01%~7.86%和3.18%~7.03%,检出限为0.1 μg/kg,定量限为0.3 μg/kg。实际样品测定结果分别为:双酚A 2.4~3.8 μg/kg;双酚S 0.48~0.82 μg/kg。本方法前处理简单、高灵敏度适用于全蛋粉中双酚A和双酚S的日常测定。     

高压液相色谱法测定大豆异黄酮含量

大豆试样在酸性条件下水解后,采用岛津LC-10AtvpHPLC仪,紫外检测器(SPD-10Avvp),波长 254 nm,色谱柱:Inertsil ODS-3柱(5μm,4.6 mm×250 mm),流动相:甲醇:5％ 醋酸溶液30％～70％梯度洗脱,流速:1.0 ml/min,柱温:50℃条件下,测定水解提取物中大豆异黄酮含量。测定结果表明:不同品种、产地的大豆中异黄酮含量为 1.40 mg～3.30 mg/g,大豆胚芽中异黄酮含量最高,为13.18mg/g;其它豆类,如红豆、绿豆、青豆、豌豆等异黄酮含量为0.37mg～1.2mg/g,此测定法能为大豆的选育种、栽培及大豆异黄酮含量评价提供依据。     

Determination of Synthetic Colors in Soft Drinks and Confectioneries by Micellar Electrokinetic Capillary Chromatography

A method of micellar electrokinetic capillary chromatography (MEKC) was developed for simultaneous determination of 14 synthetic colors in soft drinks and confectioneries. The optimal solvent of MEKC method for separating all colors was a mixed solution comprised of 18% acetonitrile and 82% 0.05 M sodium deoxycholate in borate‐phosphate buffer (pH 7.8). These colors were well separated within 20 min using 57 cm × 75 micrometer uncoated fused‐silica capillary column, operating at 25 kV and detected by UV at 214 nm. The average recovery of all colors spiked into soft drinks and confectionery was better than 82%. The addition of illegal colors was not found after testing 30 samples. In retail foods, the colorant found in highest concentration was tartrazine (155 μLgg/g sample).     

高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量

建立高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量的方法。均质后的样品用乙酸乙酯提取,稀盐酸反萃取,正己烷脱脂,荧光胺衍生,反相色谱柱分离,荧光检测器检测,磺胺5-甲氧嘧啶为内标物,内标法定量。4种磺胺类药物磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶和磺胺甲基异噁唑的线性范围为0.01～0.2mg/kg,线性相关系数均大于0.9934;在0.01～0.2mg/kg 范围内四个添加水平范围内的平均回收率为83.0%～91.3%,相对标准偏差为3.89%～8.80%,方法检出限为0.01mg/kg。     

Determination of Biogenic Amines in Pu-erh Tea with Precolumn Derivatization by High-Performance Liquid Chromatography

In recent years, Pu-erh tea is popular around the world particularly due to its special health benefits. However, biogenic amines and their safe concentration in Pu-erh tea have not been fully studied. Therefore, we selected 28 kinds of Pu-erh tea from Yunnan Province, China, to determine methylamine, ethylamine, tryptamine, putrescine, cadaverine, histamine, tyramine, and spermidine contents. The analytical method involved an extraction with hydrogen chloride solution, precolumn derivatization of the amines with dansyl chloride, and subsequent analysis by high-performance liquid chromatography with UV detection. The relative correlation coefficient of this method was greater than 99%. Limits of detection were found between 0.2 and 1.1 μg/L. Recovery rates varied from 85 to 104%. Relative standard deviations were below 5%. Additionally, this study measured the concentrations of eight biogenic amines in Pu-erh tea using pure water extractions. The predominant amines in Pu-erh teas are methylamine, ethylamine, and tryptamine. The quantities of biogenic amines in the Pu-erh teas analyzed did not exceed established international safety limits for other food or beverages, and thus, Pu-erh teas appear to be safe to drink in this respect.     

高效液相色谱法测定保健食品和饮料中维生素C

目的建立保健食品及饮料中维生素C的高效液相色谱检测方法。方法ODS C18 5μm反相色谱柱分离,流动相和试样提取液为0．1％草酸溶液。紫外检测器,流速1．0ml／min,检测波长262nm。结果线性范围为0．05—700．00μg／ml。加标回收率为84．2％-94．9％,RSD〈10％,检出限为0．05 μg／ml。结论本方法操作简便、快速、数据可靠,适合于饮料及保健食品中的维生素C含量测定。     

Development of a Precolumn Derivatization Procedure Prior to Ultrasound-Assisted Cloud Point Extraction for Sensitive Determination of Fluoroquinolones in Eggs by High-Performance Liquid Chromatography with Fluorescence Detection

In this work, a 4-chloro-7-nitrobenzodioxazole (NBD-Cl) derivatization coupled with the ultrasound-assisted cloud point extraction (UACPE) method prior to high-performance liquid chromatography with fluorescence detection (HPLC-FLD) analysis was developed for the determination of four widely used fluoroquinolones (FQs) including norfloxacin (NOR), ciprofloxacin (CIP), sarafloxacin (SAR), and gatifloxacin (GAT) in eggs. The derivatives of FQs with NBD-Cl were extracted into the Triton X-114 surfactant-rich phase, which was analyzed by reversed-phase HPLC-FLD. Ultrasound was applied to accelerate the phase separation in extraction and enhance the extraction efficiency of target analytes. Variable parameters affecting the derivatization and UACPE procedure were systematically evaluated and optimized. Under the optimum conditions, four FQs were successfully separated within 30 min through an Agilent TC-C₁₈ column. Good recoveries of 86.2–103.5 %, which were calculated using a range of spiked samples at three concentrations, were obtained by UACPE. The calibration graphs were linear over the range of 1.2–73.0 μg kg^?1 for four FQs with correlation coefficients (R) no less than 0.9957. The limits of detection were 0.2, 0.5, 0.3, and 0.4 μg kg^?1 for NOR, CIP, SAR, and GAT, respectively. The precisions indicated by relative standard deviations ranged from 0.6 to 4.3 % for both intraday and interday analysis. The proposed method proved to be a selective, sensitive, and eco-friendly approach which was successfully applied to analyze FQs in eggs at the local farmers market, and none of the target analytes were detected in these samples.     

Determination of 13 Phenolic Compounds in Rice Wine by High-Performance Liquid Chromatography

Rice wines are widely consumed by the general public in Asian countries, while comprehensive studies focused on the individual phenolic compounds in rice wines are limited. A rapid method for simultaneous determination of 13 phenolic compounds in rice wines by high-performance liquid chromatography (HPLC) was developed and validated, and the phenolic compounds in commercial rice wine samples (Chinese rice wine, Japanese sake, and Korean makgeolli) were determined in this paper. The identified compounds contained gallic acid (GA), protocatechuic acid (PRCA), vanillic acid (VA), syringic acid (SRA), caffeic acid (CA), ferulic acid (FA), p-coumaric acid (pCA), sinapic acid (SA), chlorogenic acid (CHA), (+)-catechin (CAT), (?)-epicatechin (EPI), quercetin (QUE), and rutin (RUT). Phenolics were separated with a C18 reversed-phase column at 38 °C by gradient elution using 3 % acetic acid aqueous solution (solvent A) and acetonitrile (solvent B) (0 min, 5 % B; 5 min, 8 % B; 10 min, 15 % B; 20 min, 25 % B; and 25 min, 5 % B) as the mobile phase at 280 nm with flow rate of 1.0 mL min^?1. With direct injection of rice wine samples, the chromatograms of all analytes were observed within 20 min, all calibration curves were linear (R ²?>?0.995) within the range, limits of detection (LOD) ranged from 0.02 to 0.06 μg mL^?1, and good recoveries (88.07–106.80 %) and precision (relative standard deviation (RSD)?<?5.36 % ) were obtained for all compounds. This method was applied to quantify phenolic compounds in commercial rice wine samples (Chinese rice wine, Japanese sake, and Korean makgeolli), and good separation peaks were observed and catechin was the predominant phenolic in the samples. The average values of total phenolic contents of the three groups of rice wine were significantly different (p?<?0.01). In conclusion, this procedure can be used to determine the phenolic compounds in various types of rice wines, as well as to characterize and differentiate rice wine samples.     

柱前衍生反相高效液相色谱法测定干酪中生物胺的含量

用所建立的反相高效液相色谱-荧光检测法测定干酪中的生物胺。采用的色谱柱为HP Hypersil ODS柱(125mm×4．6mm×5μm);荧光检测激发波长为340nm,发射波长为450nm;洗脱程序为梯度洗脱,流速为1．0ml/min。干酪样品经邻苯二甲醛柱前自动衍生,能使组胺、酪胺、腐胺、尸胺、色胺在15min内得到良好分离,并且各生物胺浓度在0．01～25mg/L时其浓度与相应峰面积有良好的线性关系,最低检测限(以信噪比为3计)为0．005～0．01mg/L。样品加标各生物胺的回收率为92．6%～107．4%。该法快速准确、简便灵敏、分离度高,能够满足干酪中生物胺的检测要求。