QuEChERS-超高效液相色谱-串联质谱法快速测定辣椒红色素中9种非食用色素

采用QuEChERS前处理方法,结合超高效液相色谱-串联质谱多反应监测模式下的定性和定量分析,实现辣椒红色素中9种非食用色素的同时检测。辣椒红色素样品经乙腈溶液提取后,氯化钠进行盐析,C18吸附剂净化,取上清液进行超高效液相色谱-串联质谱分析。方法的基质效应影响在-0.17～0.07之间,检出限在0.2～1.5 ng/g之间,定量限在0.6～5.0 ng/g之间,碱性橙II、碱性橙21、碱性橙22、碱性嫩黄在0.2～8 ng/mL范围内线性关系良好,苏丹红I、苏丹红II、苏丹红III、苏丹红IV、罗丹明B在2～40 ng/mL范围内线性关系良好,目标物线性相关系数R2均大于0.995 0,9种非食用色素在3个样品加标水平的平均回收率均在69.6%～92.5%之间,相对标准偏差在2.8%～8.5%之间(n=5)。该方法简单快捷、准确可靠,适合于大批量天然植物提取物样品中非食用色素的快速检测。     

采用微型GPC柱快速筛查辣椒制品中非食用色素

建立了一种采用微型凝胶渗透色谱(gel permeation chromatography, GPC)柱筛查辣椒制品中脂溶性非食用色素的方法,采用普通玻璃滴管装填Bio-Beads S-X3凝胶制备微型GPC柱(10 cm× 0.5 cm, i.d.),样品经有机溶剂提取,以正己烷/乙酸乙酯(1∶1,v/v)或环己烷/乙酸乙酯(1∶1,v/v)为流动相,对样品提取液进行柱层析筛查,通过肉眼观察被检样品在凝胶柱中是否分离出保留时间(或保留体积)与非食用色素标准品一致的新色素带,判断样品中是否含非食用色素.该筛查方法操作简便、成本底,结果直观、准确,具有较大的推广应用价值.     

超声辅助提取-液相色谱-串联质谱法同时测定马卡龙中人工合成色素与天然色素

目的建立超声辅助提取-液相色谱-串联质谱法同时测定马卡龙中的8种人工合成色素与天然色素。方法样品在60%的乙醇水溶液中,使用超声辅助方式提取色素,提取液过滤后直接采用液相色谱-串联质谱法进行检测,基质外标法进行定量。结果在较宽的线性范围内,线性关系良好(r~20.99);在3个添加水平下,回收率在80.3%～103.7%之间,且相对标准偏差均小于15%;8种色素的检出限为0.27～0.84mg/kg,定量限为0.9～2.6 mg/kg。结论该方法快速、简便,灵敏度较高,适用于马卡龙中人工合成色素与天然色素的测定。     

UPLC-MS-MS法检测辣椒及其制品和肉酱中的罗丹明B含量

建立了辣椒及其制品和肉酱中罗丹明B含量的超高效液相色谱-串联质谱联用检测方法。样品经乙腈提取后,经中性氧化铝固相萃取柱净化,超高效液相色谱-串联质谱法检测。本方法定量限0.1μg/kg,线性范围0.2~50 ng/mL;在罗丹明B添加水平0.1~10μg/kg时,辣椒片样品中的回收率76%~92%,辣椒制品中的回收率74%~93%,肉酱样品中的回收率70%~90%。     

食品接触材料及制品中芳香胺毒性与检测方法研究进展

综述了20种芳香胺的毒性、国内外对其在食品接触材料及制品中迁移的相关法规及检测标准,并讨论对比了气相色谱法、液相色谱法、液相色谱-质谱法、气相色谱-质谱法、实时直接分析质谱法五种检测方法的定量限、检出限、加标回收率等指标。     

UPLC-MS/MS测定食品中18种非食用色素的研究

建立以超高效液相色谱-串联三重四级杆质谱同时测定辣椒酱中18种非食用色素的有效方法。样品通过MgSO4和NaCl协同乙腈振荡提取,提取液经QuEChERS(quick、easy、cheap、effective、rugged、safe的简称)填料净化后采用多反应监测(multiple reaction monitoring,MRM)模式进行测定。结果表明:18种非食用色素的定量限为6.0μg/kg～51.0μg/kg,回收率为80.2%～109.2%,相对标准偏差为2.4%～9.7%。该方法实现了多种非食用色素的同时分析,适用于打击辣椒酱中非法添加非食用色素的快速检测。     

固相萃取-高效液相色谱-串联质谱联用法检测辣椒及其制品和肉酱中的罗丹明B含量

建立了辣椒及其制品和肉酱中罗丹明B含量的固相萃取-高效液相色谱-串联质谱联用(SPELC-MS/MS)检测方法。样品经乙腈提取后,经中性氧化铝固相萃取柱净化,超高效液相色谱-串联质谱法检测。本方法定量限为0.1μg/kg,线性范围为0.2~50ng/mL;在罗丹明B添加水平为0.1~10μg/kg时,辣椒片样品中的回收率为76%~92%,辣椒制品中的回收率为74%~93%,肉酱样品中的回收率为70%~90%。     

液相色谱-串联质谱法测定芦荟苷方法的建立

建立液相色谱-串联质谱法测定芦荟苷的方法,采用ESI负离子模式,多反应监测测定芦荟苷的分子离子峰为417.2,定量离子为297.2,定性离子为268.2和250.2;对方法进行验证,液相色谱-串联质谱法测定芦荟苷的线性R=0.999 4,出限为1.0 nμg/L,精密度RSD≤3%,是一种理想的检测方法,为芦荟制品质量检测、食品风险评估、合成分析研究、代谢研究提供数据及技术手段。     

湖南常见辣椒品种游离氨基酸主成分分析及综合评价

游离氨基酸参与辣椒中风味物质的合成,其种类及含量与辣椒品种密切相关.采用高效液相色谱-串联质谱法对湖南常见大红椒、青尖椒、螺丝椒、小米椒、小红椒、大青椒6种辣椒的游离氨基酸进行分析,明确不同辣椒品种游离氨基酸组成差异,以期为合理开发和利用辣椒资源提供理论依据.结果表明:6种辣椒中共检出24种游离氨基酸,其中青尖椒、螺丝...     

超高液相色谱串联质谱法检测土豆及土豆制品中α-茄碱

目的建立超高效液相色谱串联质谱法检测土豆及其制品中α-茄碱的分析方法。方法通过优化提取液,土豆样品经1%甲酸-甲醇(1:1,V:V)超声提取,采用BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm)分离,梯度洗脱,采用超高效液相色谱串联质谱法,在多反应监测模式进行定性和定量分析,而土豆淀粉用MCX固相萃取柱进行净化,液相色谱串联质谱法测定。结果土豆样品中回收率为75%~115%,相对标准偏差为5.0%~8.6%,土豆淀粉的回收率范围为67%~100%,相对标准偏差为3.4%~11.3%,方法的检出限和定量限分别为0.5 mg/kg和1.0 mg/kg。结论该方法适合于土豆及其制品中α-茄碱的分析。     

色谱质谱技术在食品安全分析检测中的应用

食品安全是关系国计民生的重要议题。准确、深入、高效的食品安全分析检测技术是防控食品安全事件发生及处理相关贸易纠纷、立法追责的基础和保障。色谱质谱技术作为高效的分离和检测手段是目前食品安全分析领域最重要、最主流的技术手段。近年来,色谱质谱领域的新发展也推动了食品安全分析检测向更快速,更有效,更可靠,更安全的目标迈进,本综述就其中最重要并有望代表未来食品安全分析发展趋势的色谱质谱技术做了总结和点评。如用于食品样品预处理的固相微萃取技术;气相色谱及气相色谱质谱联用技术中的快速气相色谱方法及其与质谱联用方法,二维气相色谱方法及其与质谱联用方法;液相色谱及液相色谱质谱联用技术中的超高效液相色谱及其与质谱联用方法,毛细管液相色谱和纳流液相色谱及其与质谱联用方法,超临界色谱及其与质谱联用方法,二维液相色谱及其与质谱联用方法;质谱分析技术中的超高分辨率质谱方法,常压敞开式离子源质谱技术等。     

Synthesis and chemical characterisation of curcuminoid colouring principles for their potential use as HPLC standards for the determination of curcumin colour in foods

The three major colour principles of curcumin have been synthesized, purified and chemically characterized using nuclear magnetic resonance spectroscopy, absorption spectroscopy, high- performance liquid chromatography and liquid chromatography-mass spectrometry. System suitability criteria for the simultaneous determination of the curcuminoids and annatto colorant (bixin and norbixin) by HPLC are presented and the importance of the water content of sample extracts discussed. The results show that synthetic curcuminoids may be synthesized with sufficient purity for use as standards for HPLC analysis provided that both the spectrophotometric and chromatographic purities are known. The potential for their use in the determination of turmeric and/or added curcumin colour (with annatto) in foods and especially fish is discussed.     

A new analytical method for gonyautoxins based on postcolumn HPLC

A new ion-pairing high-performance liquid chromatography (HPLC) method on a C30 column with a volatile mobile phase was developed to separate the gonyautoxin group (GTXs) from contaminants, allowing the utilization of liquid chromatography/mass spectrometry (LC/MS) with higher performance. A mobile phase consisting of 5 mmol/L heptafluorobutyric acid and 2% acetonitrile in 10 mmol/L ammonium acetate was adopted for separation of GTXs because the C30 column strongly retains GTXs under acidic conditions. The newly adopted method could efficiently separate GTXs from contaminants, especially in the toxic short-necked clam, whereas the routine HPLC so far used has poor resolution to separate GTXs from unknown interfering substances. In our method, GTXs were eluted in the order of GTX5, GTX3, GTX4, GTX2 and GTX1 from the C30 column, and were successfully determined by sonic spray ionization mass spectrometry (SSI-MS) with high sensitivity. This method is characterized by the combination of HPLC using a fluorescence detection system for PSP, and SSI-MS for measurement of the mass number.     

高效液相色谱-离子阱-飞行时间质谱法定性分析蜂蜜中的黄酮类未知物

目的 建立高效液相色谱-离子阱-飞行时间串联质谱法(high performance liquid chromatography-ion trap-time of flight tandem mass spectrometry, HPLC-MS-IT-TOF)定性分析蜂蜜中的未知黄酮类物质的分析方法。方法 通过查阅相关资料, 推断该未知物可能是黄酮类物质, 用质谱检测可知与其他干扰物质是否分离。在确定干扰物质与未知黄酮进行分离后, 可以得到未知黄酮类物质的分子离子峰和三级质谱碎片, 根据碎片离子, 推导出了裂解途径, 并使用分子式软件预测了未知黄酮类物质的分子式。结果 综合实验结果, 最后定性了蜂蜜中的未知黄酮类物质为“短叶松素”, 其分子式为C15H12O5。用超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)将黄酮类未知物质与短叶松素标准品的保留时间、离子对m/z 271.06＞253.10和m/z 271.06＞191.00及离子比率进行比对, 确证定性结果是准确的。结论 本实验为蜂蜜中黄酮类未知物定性提供了一个有效的思路和方法。     

Deodorization of a Colorant Prepared from Red Cabbage

A process for preparing odor-free colorant from red cabbage was developed. Anthocyanins in an acidified aqueous cabbage extract were adsorbed on Amberlite XAD-7, water-washed to remove residual cabbage odor, eluted with ethanol containing 0.1% HCl, and concentrated by evaporation. Optimal conditions for single stage batch contact and column deodorization were determined. Pigment recovery generally exceeded 90%. The stability, spectral, and colorant properties of the recovered pigments were not altered significantly by the process. Spent adsorbent could be regenerated by water washing without adversely affecting process efficiency or colorant performance.     

Prediction of the amino acid composition of small peptides contained in a plant protein hydrolysate by LC–MS and CE–MS

An original procedure is described to propose the amino acid composition of small peptides (molar mass < 1000 g/mol) contained in a complex vegetable protein hydrolysate. This method is based on two predictive models: the first is related to the peptide hydrophobic character using reversed-phase liquid chromatography–mass spectrometry analysis; the second to the peptide charge-to-mass ratio using capillary electrophoresis–mass spectrometry analysis. A software has been developed to determine the possible amino acid combinations as a function of the mass determination and of the data provided by both models. This computer-aided method has been applied to a rapeseed protein hydrolysate. In the hydrolysate, the amino acid sequence of some unknown vegetable peptides has been determined, using the sequences of native proteins.     

HPLC–MS analysis of the green food colorant sodium copper chlorophyllin

Five commercial samples of sodium copper chlorophyllin, a green food colorant, were analysed by high-performance liquid chromatography (HPLC) using diode-array detection (DAD) and mass spectrometry (MS). Some of the constituents were identified using authentic standards, whereas others were identified tentatively based on their absorption spectra and mass data. The composition of three of the samples was very similar, whereas the other two were quite different. In the three former samples, the three largest peaks could be assigned to Cu chlorin e₆, Cu chlorin p₆, and Cu isochlorin e₄. In one of the two other samples, these three compounds were also among the largest peaks, whereas Cu chlorin e₆ was a small peak in the last sample and Cu chlorin p₆ was absent altogether. Porphyrins were also present in the samples, while except in one of the samples chlorins derived from chlorophyll b were largely absent.Industrial relevanceSodium copper chlorophyllin is a green food colorant made from chlorophyll. Sodium copper chlorophyllin is made by saponifying chlorophyll and coppering the resulting product. This processing leads to a complex mixture of compounds. An analytical method was developed that can be used to identify many of these compounds and show the extent of coppering and degradation of sodium copper chlorophyllin, which may be used industrially to optimize the production of sodium copper chlorophyllin.     

液相色谱和液质联用法分析食品中苯并咪唑类药物残留的研究进展

苯并咪唑类药物作为驱虫剂和杀菌剂广泛使用,该类组分及其代谢物引起的食品安全问题得到越来越多的关注。液相色谱与液相色谱质谱法是目前检测食品中苯并咪唑类物质的常用方法,本文汇总了苯并咪唑类物质主要用途以及残留标志物等基本信息,论述了QuEChERS技术、固相萃取技术、液-液萃取技术以及分子印迹技术四种前处理方法,总结了液相色谱以及液质联用在检测食品中苯并咪唑上的应用,建议通过提高设备的小型化和自动化、精准前处理吸附剂材料以及完善质谱数据库来提高苯并咪唑类物质的检测水平,旨在为食品中苯并咪唑类物质检测的深入研究提供参考。     

UPLC-MS/MS法同时测定豆芽中氟喹诺类药物和生长调节剂

目的? 采用GCB、Z-sep+等净化材料改进的QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)建立一种能够快速、稳定地同时测定豆芽中多种喹诺酮类以及生长调节剂药物残留的分析方法。 方法 样品粉碎,经甲酸乙腈提取,净化包材料净化后,通过保留时间匹配以及母离子、主要碎片离子的精确质量数进行定性分析、基质标准溶液外标定量的方法进行分析。结果 在优化条件下, 9种参数的保留时间在4.9~8.8 min。质量浓度范围在0.010~0.200μg/mL时, 9种参数的线性关系良好, 其相关系数为0.9149～0.9999之间, 检出限(LOD)达到5.0μg/kg,定量限(LOQ)达到10μg/kg。结论 试验方法操作简单、准确, 可快速定性定量分析豆芽中9种氟喹诺类药物和生长调节剂的残留,对实现豆芽种植过程管控、日常监管、质量保障具有重要意义。     

Identification of Antioxidants in Aged Garlic Extract by Gas Chromatography-Mass Spectrometry and Liquid Chromatography-Mass Spectrometry

A novel aged garlic extract, with high antioxidant activities, was prepared by soaking sliced garlic in 10% ethanol solution for 90 days. In order to locate the antioxidant ingredients of aged garlic extract, 2,2-azinobis-6-s (3-ethylbenzothiazoline sulfonic acid) assay, hydroxyl free radical assay, 2,2-diphenyl-1-picrylhydrazyl assay, and ferric reducing/antioxidant power assay were conducted to guide the fractionation of aged garlic extract by means of extraction. As a result, the ethyl acetate fraction was identified as the highest antioxidant activity in aged garlic extract. Therefore, the ingredient information of the ethyl acetate fraction were obtained through gas chromatography–mass spectrometry and ultra performance liquid chromatography mass spectrometry / mass spectrometry analysis. Some phenols and diallyl disulphide, 5-(hydroxymethyl)-2-furancarboxaldehyde, S-allyl-cysteine, S-allyl-mercaptocysteine, and 1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid were identified as potent antioxidants in aged garlic extract by gas chromatography–mass spectrometry and ultra performance liquid chromatography mass spectrometry / mass spectrometry, respectively. The biological activities and formation mechanisms of these identified compounds were discussed.