高效液相色谱- 电喷雾三级四极杆质谱测定苹果、山楂、番茄制品中棒曲霉素的研究

建立了苹果、山楂、番茄制品中棒曲霉素总量的提取方法和液相色谱串联质谱确证方法。清汁样品用乙腈稀释后直接过MycoSep 228 真菌霉素多功能净化柱;浊汁、固体样品用果胶酶水解后,再用乙酸乙酯提取样品中棒曲霉素,浓缩后经MycoSep 228 柱净化,用Atlantis dC18 色谱柱分离,液相色谱串联质谱测定,电喷雾负离子(ESI －)多反应模式下监测;实验结果表明,样品中棒曲霉素浓度在1.0～200μg/kg 范围内时与其峰面积成良好线性关系,检测低限为2.0μg/kg,3 个加标水平下回收率为76.0%～95.3%,相对标准偏差为5.4%～11.2%。该方法选择性好,灵敏度高,定性可靠,可满足苹果、山楂、番茄制品中棒曲霉素测定的要求。     

QuEChERS/HPLC-MS法测定食品中的生物碱

采用QuEChERS/HPLC-MS法测定食品中罂粟碱、那可丁、蒂巴因、可待因、吗啡等五种生物碱,方法简便,准确度符合要求.吗啡、可待因用内标法定量,罂粟碱、那可丁和蒂巴因用外标法定量.经计算,加标回收率满足要求.     

A LC-HRMS After QuEChERS Cleanup Method for the Rapid Determination of Dye Residues in Fish Products

The reliability of a rapid LC-HRMS method was studied in order to find a sensitive and accurate, simple, cheap, and rapid method for screening and quantitative determination of malachite green (MG), leucomalachite green (LMG), brilliant green (BG), crystal violet (CV), and leucocrystal violet (LCV) in fish muscle. All the analytes were extracted using a mixture of acetonitrile and citrate buffer, while the cleanup phase was carried out by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. All the data analyzed were acquired using both full MS and dd-MS² modes. Good specificity, precision (relative standard deviation <11% for each sample tested), recovery (10–60%), decision limit (CCα between 0.55 and 0.62 μg kg^?1), detection capabilities (CCβ between 0.65 and 0.78 μg kg^?1), and ruggedness were achieved for the reliability of the method. Satisfactory results were obtained during the linearity test in the range of 0.10–2 ng mL^?1 (r ² > 0.999). Best recoveries were obtained by the QuEChERS cleanup method for all the analytes examined, presenting values between 70 and 104%. The application of 70,000 FWHM mass resolution and narrow mass windows significantly improved the selectivity of the method, leading to simultaneous screening and quantification of dye residues in comparison to other methods proposed in literature. The optimized method proposed in this work enables a simple and fast preparation; it offers exceptional sensitivity and selectivity and maximizes efficiency and reproducibility with a low consumption of reagents. Finally, the present method was successfully employed to detect dye residues in 73 fish samples, as provided for the national residue control plan.     

Optimization and Validation of a Method Without Alkaline Clean-Up for Patulin Analysis on Apple Puree Agar Medium (APAM) and Apple Products

A sensitive high-performance liquid chromatography-UV (HPLC-UV) method, based on the Association of Analytical Communities (AOAC) Official method 2000.02, was developed and validated for the high-throughput analysis of patulin in in vitro experiments on apple puree agar medium (APAM). The importance of repeating the ethyl acetate extraction step at liquid-liquid extraction (LLE) was examined, as well as the extent of patulin degradation during the sodium carbonate clean-up. In addition to this alkaline clean-up, the efficiency of using an Oasis HLB or C₁₈ cartridge as solid-phase extraction (SPE) clean-up was compared. This resulted in a two-step ethyl acetate LLE, followed by an Oasis HLB SPE clean-up, without alkaline clean-up conditions. The method was fully validated for APAM, cloudy apple juice, and apple puree. Average patulin recoveries at levels of 100, 500, and 1000 μg kg^?1 of APAM varied between 95 and 113 % over 3 independent days, with an interday precision (RSD_R) of 5 to 10 %. Recovery experiments carried out with the spiked apple juice (at 50 μg kg^?1) and apple puree (10 μg kg^?1) showed average recovery rates laying between 80–101 % (RSD_R?=?12 %) and 77–100 % (RSD_R?=?9 %), respectively. This method offered a detection limit of 3–4 μg kg^?1 and a quantification limit of 5–8 μg kg^?1 for APAM, apple juice, and puree.     

QuEChERS 在食品中农药多残留检测的应用研究进展

食品中农药残留的检测是一项关系到食品安全的重要问题,而前处理是农药残留检测中耗时最长、工作量最大的部分,前处理质量的好坏决定着分析的准确性和精密度。QuEChERS方法由于具有快速、简单、廉价、有效、可靠、安全的特点成为一种备受关注的样品前处理新技术。本文就QuEChERS方法在水果、蔬菜、粮谷、动物食品等农药多残留控制检测的应用研究中取得的成果和发现的问题进行综述,对以后的发展作一展望。     

采用ICS3000型离子色谱法对苹果汁中棒曲霉素含量的测定

采用离子色谱法对苹果汁中棒曲霉素含量的测定,棒曲霉素主要来源于青霉病,此病危害成熟或接近成熟的果实,病斑黄白色,近圆形,果肉腐烂呈锥状湿腐,当条件适宜时,使全果腐烂,产生强烈的霉味同类标准执行的是苹果汁中的棒曲霉素最大限量50μg/L。美国戴安公司生产ICS300离子色谱,Ultimate 3000 varible waveleng detector紫外检测器。旋转蒸发仪、一次性滤膜0.45μm、1～5、5～10mL加样枪,色谱柱Diamonsil 5uc18 250×4.6mm,美国密理博公司生产的Direct-Q3超纯水机。     

苹果汁中展青霉素和羟甲基糠醛的高效液相色谱测定方法

为了建立能有效地将苹果汁中羟甲基糠醛分离的展青霉素高效液相色谱测定方法,将苹果汁样品用乙酸乙脂提取,提取液经碳酸钠溶液净化,无水硫酸钠脱水,再通过反相色谱柱检测。色谱柱为supelco C18柱,紫外检测器检测波长为275nm。结果表明:展青霉素和羟甲基糠醛能完全分离,其检出限均为5μg/L,加标回收率分别为73.1％～82.7％和78.8％～83.6％。从而建立了一个能有效分离羟甲基糠醛的准确、灵敏的展青霉素高效液相色谱测定方法。     

苹果及其制品中展青霉素生物防治研究进展

展青霉素是一种由真菌产生的次级代谢产物,普遍存在于腐烂的蔬菜、水果中,特别是苹果及其制品中。展青霉素具有广泛的生理及细胞毒性,对人的健康和安全构成了严重的威胁。近年来,采用生物防治方法控制苹果及其制品中展青霉素的污染已成为国际学术界研究的热点。本文综述生物防治方法控制苹果及其制品中展青霉素的研究进展,并论述展青霉素的生物防治机制,为推动生物防治方法在展青霉素控制方面的应用提供参考。     

QuEChERS前处理方法在食品检测中的应用进展

样品前处理是食品检测中的关键步骤,QuEChERS技术具有快速、简便、便宜、高效、可靠、安全等优点,不仅广泛应用于水果、蔬菜、谷物等样品中农药残留检测,还广泛应用于兽药残留、毒素、污染物、非法添加物等物质的检测,且涵盖的样品基质也越来越多。该文对近些年QuEChERS技术的改进以及在食品领域的应用进行综述。     

固相萃取-高效液相色谱法测定苹果汁及其饮料中展青霉素的含量

建立固相萃取-高效液相色谱法测定苹果汁及其饮料中展青霉素含量的检测方法。样品经预处理后,采用固相萃取柱净化处理,以乙腈-水作为流动相,C18色谱柱分离,二极管阵列检测器进行检测。结果表明：方法检出限为8 μg/kg,方法定量限为25 μg/kg;展青霉素标准溶液在50.0～500.0 μg/L质量浓度范围内,决定系数R2为0.999 6;样品中展青霉素含量为25～100 μg/kg时,回收率在90.2%～102.8%之间,精密度（变异系数）为0.57%～1.44%。此方法准确度较高,成本适中,操作较简便,适合苹果浓缩汁生产企业用于产品安全自控。     

高效液相色谱法测定浓缩苹果汁中棒曲霉毒素

利用全自动凝胶渗透色谱净化系统净化、在线浓缩样品,采用高效液相色谱分离,紫外检测器检测建立了浓缩苹果汁中棒曲霉毒素的检测方法。样品经乙酸乙酯:环己烷(1:1)提取,凝胶渗透色谱(GPC)净化,在线浓缩并定容,采用C18柱分离,以乙腈:水(体积比为10:90)为流动相,流速1.0ml/min;检测波长276nm。浓度0.01～10.0mg/L时线性关系良好,加标回收率为83%～107%,相对标准偏差为7.8%～11.4%,检出限0.005mg/kg。该方法操作简单、灵敏度高、重复性好。     

固相萃取-离子对液相色谱法测定保健品中的叶酸

建立了一种快速、准确、灵敏的固相萃取- 离子对反相高效液相色谱测定保健品中叶酸的方法。用Chromabond-SB 萃取小柱富集保健品中的叶酸,以四丁基溴化铵为离子对试剂,优化了色谱条件。采用 Lu-Na C18色谱柱(250mm × 4.6mm,5μm),SPD-6AV 紫外可见吸收检测器,流动相为0.05mol/L KH2PO4-0.01mol/L 四丁基溴化铵- 乙腈(88:2:10,V/V),用磷酸调节 pH5.5,流速 1.0ml/min,检测波长284nm。结果表明：叶酸在0.06～2.40μg/ml 浓度范围内,峰面积和浓度呈良好的线性关系,相关系数为0.9996,最小检出限为0.008μg/ml,加标回收率为 95.14%～102.87%。     

A New and Fast HPLC Method for Determination of Rutin, Troxerutin, Diosmin and Hesperidin in Food Supplements Using Fused-Core Column Technology

A new and fast high-performance liquid chromatography (HPLC) method using fused-core column for separation of rutin, troxerutin, diosmin, and hesperidin has been developed and used for determination of these flavonoids in food supplements. Efficient separation of flavonoids and internal standard methylparaben was achieved on the fused-core column Ascentis Express RP-Amide (100?×?3.0 mm), particle size 2.7 μm, with mobile phase acetonitrile/water solution of acetic acid pH?3 (30:70, v/v) at a flow rate of 1.0 mL?min^?1 and at temperature 50 °C. The detection wavelengths were set at 283 nm for hesperidin and at 255 nm for rutin, troxerutin, diosmin, and internal standard methylparaben. Under the optimal chromatographic conditions, good linearity with correlation coefficients in the range (r?=?0.9991–0.9998; n?=?7) for all flavonoids was achieved. Commercial samples of food supplements were extracted with 100 % dimethyl sulfoxide using ultrasound bath for 10 min and then diluted to methanol. A 5-μL sample volume of the filtered solution was directly injected into the HPLC system. Accuracy of the method defined as a mean recovery of flavonoids from food supplement matrix was in the range 96.2–104.4 % for all flavonoids. The intraday method precision was satisfactory, and relative standard deviations of sample analysis including preparation and determination of different food supplements were in the range 0.5–3.5 % for all flavonoids. The developed method has shown high sample throughput during sample preparation process, modern separation approach, and short time (5 min) of analysis.     

Presence and Stability of Patulin in Pasteurized Apple Cider

Pasteurized apple cider produced in Georgia was surveyed for patulin. Levels from 244-3993 μg patulin/L cider were found. Eight high temperature-short time (HTST) treatments (60°, 70°. 80°, and 90°C for 10 set; 90°C for 20, 40, 80, and 160 set) and one batch treatment (90°C for 10 min) were used to determine the stability of patulin in pasteurized cider. The 60°, 80°, and 90°C HTST treatments and the batch pasteurization significantly reduced the patulin level, but did not completely destroy the toxin. Storage of the cider had no effect on the patulin level.     

Comparing d-SPE Sorbents of the QuEChERS Extraction Method and EMR-Lipid for the Determination of Polycyclic Aromatic Hydrocarbons (PAH4) in Food of Animal and Plant Origin

A Quick, Easy, Cheap, Rugged, Effective, and Safe (QuEChERS) method for the determination of benzo[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[a]pyrene (PAH4 including the interfering PAHs triphenylene, cyclopenta[c,d]pyrene, benzo[k]fluoranthene, benzo[j]fluoranthene) was developed and validated with GC-MS/MS in foods of plant and animal origin. PAHs were extracted with acetonitrile, and different clean-ups with various compositions of sorbents, including zirconia-based sorbent (Z-Sep), primary-secondary amine (PSA), anhydrous magnesium sulfate (MgSO₄), octadecylsilane (C18 endcapped), and enhanced matrix removal (EMR)-lipid material, were tested. Another important focus of this study was the separation of critical pairs, which is essential for the qualification and quantification of PAH4. To investigate the developed methods, samples were spiked beneath their maximum levels (MLs) and recoveries and peak shapes were compared. The clean-up with 900 mg MgSO₄ + 150 mg PSA + 150 mg C18 was chosen to be validated in salmon, mussels, shrimps, bacon, cutlets, wheat flour, curry spice powder, infant formula, infant follow-up formula, and infant foods. Recoveries for all analytes were between 75 and 108%, combined with standard deviation between 2 and 20%. Limits of detection (LODs) and limits of quantification (LOQs) were between 0.04 and 0.34 μg/kg and between 0.1 and 1 μg/kg, respectively.     

核固红光度法测定乳制品中微量铬

建立核固红光度法测定乳制品中微量铬的新方法。在盐酸介质中,铬(Ⅵ)能够氧化核固红而使溶液褪色,且褪色程度与铬(Ⅵ)的质量浓度在一定范围内呈线性关系,据此可以测定铬(Ⅵ),若将铬(Ⅲ)在NaOH溶液中以H2O2氧化成铬(Ⅵ),即可测定总铬,实现铬(Ⅵ)与铬(Ⅲ)的同时测定。在最大吸收波长560nm处,Cr(Ⅵ)的质量浓度在0.2～1.6µg/mL范围内符合比尔定律,表观摩尔吸光系数为2.2×104L/(mol·cm)。方法用于几种乳制品中Cr(Ⅲ)和Cr(Ⅵ)的同时测定,结果与二苯碳酰二肼光度法测定结果一致。     

Determination of Rhodamine B in Food Using HPLC-UV Method

[Objective]The aim was to establish a method for the determination of Rhodamine B in food by HPLC-UV.[Method]Rhodamine B was extracted with acetone/hexane from ...     

Evaluation of the QuEChERS Method with GC-MS Detection for the Determination of Organochlorine Pesticides in Food of Animal Origin

This paper reports the evaluation of the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for the determination of organochlorine pesticide residues in food of animal origin with gas chromatography–mass spectrometry detection. There is a very little information about sample preparation method for the determination of pesticide residues in food of animal origin in the literature. Moreover, any example of application of the QuEChERS method for the determination of pesticide residues in food of animal origin has not been reported as yet. The results showed that the best recovery ratios from 75 to 112 % were obtained for the method with primary secondary amine, C₁₈ sorbents and evaporation to dryness and dissolving the residues in hexane with relative standard deviation lower than 10 % for most compounds. The limit of quantification ranged from 0.0015 to 0.0071 mg kg^?1. This method was also used for the determination of pesticide residues in 15 samples of pork ham. In 12 samples, low concentrations of DDT or its metabolites and isomers of hexachlorocyclohexane were detected. Heptachlor epoxide and α-chlordane were determined in one sample and HCB in two samples. There were no exceedances of maximum residue levels (MRLs) for the determined pesticides in any of the analysed samples.     

Determination of Carbendazim in Food Products Using a Sequential Injection Analysis Optosensor

Carbendazim (CBZ) is a widely used broad-spectrum benzimidazole fungicide used to control plant diseases in cereals, vegetables, and fruits. It has been recently found that it is useful for the control of aflatoxin contamination in chili peppers (Capsicum annuum). In addition, it is useful against other diseases in peppers and tomatoes (Solanum lycopersicum). A flow-through optosensor using C₁₈ silica gel as solid support is here presented for the fluorimetric (λ _exc/λ _em?=?276/306) determination of CBZ in Capsicum powder and dried tomatoes. The proposed system has been developed using sequential injection analysis, so improving the repeatability and automation of the system and minimizing wastes generation. The method presents a detection limit of 3 μg?L^?1, a sample throughput of 16 samples per hour and interday relative standard deviation lower than 6 %. Taking into account that the maximum residue limit specified in the Codex Alimentarius for dried peppers is 20 mg?kg^?1, recovery experiments have been carried out for CBZ concentrations in the 15–40 mg?kg^?1 range, obtaining satisfactory results. Therefore, the proposed method fulfills the current legislation and could be used as an alternative to other analytical methods, such as chromatographic ones.