液相色谱-串联质谱法应用于动物源性食品中多族药物筛查确证的研究进展

为了筛查和监测动物源性食品中因不当或非法使用兽药以及一些人用药物而导致的药物残留,液相色谱-质谱联用技术成为该领域中应用最为广泛的痕量检测技术。该文从样品前处理净化方法、最新研究思路、基质效应评价、质谱检测器选取等方面对液相色谱-串联质谱法在动物源性食品中多族药物筛查确证应用的研究进展进行了综述,并对这一应用的发展前景进行了展望,希望能为相关研究的开展提供参考和启发。     

液质联用技术在蜂蜜兽药残留检测中的应用

近年来,中国蜂产品行业的快速发展,蜂蜜作为十分常见的天然动物源性食品之一,国内外消费群体对蜂蜜中兽药残留的问题越来越关注。国家监管机构也加大对此类问题的监督,由于蜂蜜基质复杂,兽药残留多处于痕量水平,因此需要较高的技术水平和仪器设备对蜂蜜中的兽药残留进行检测,高效液相色谱-串联质谱技术因其高检测精度、高灵敏度、高通量使其成为在蜂蜜中应用最广泛的技术之一,结合蜂蜜中兽药残留现状,对液相色谱-串联质谱技术在蜂蜜中兽药残留检测方法上进行阐述,并对兽药残留检测技术的发展方向进行展望。     

LC-MS/MS技术在食品中农药多残留分析的应用进展

液相色谱-串联质谱(LC-MS/MS)技术在食品中多类农药的高通量、高效率筛查和确证分析方面发挥了重要作用。本文对基于四级杆滤质器的LC-MS/MS技术近年来在食品中农药多残留分析方面的应用进展进行了综述,重点讨论了液相色谱-低分辨串联质谱(三重四级杆串联质谱和四级杆线性离子阱串联质谱)以及液相色谱-高分辨串联质谱(四级杆飞行时间串联质谱和四级杆静电场轨道阱串联质谱)在多类农药多残留分析中的应用。     

天然肠衣中兽药残留及检测方法的研究进展

近些年出口的天然肠衣多次被曝出兽药残留超标的安全问题,甚至被欧盟进行通报,因此动物源性食品的安全问题也越来越受到重视。天然肠衣基质复杂,目前国内外针对天然肠衣的兽药残留检测的研究相对较少。本文总结了国内天然肠衣中兽药残留检测相关技术的应用情况,介绍了气相色谱-质谱法、高效液相色谱法、高效液相色谱-串联质谱法、超高效液相色谱-串联质谱法、酶联免疫反应方法的研究应用进展,并展望天然肠衣中药物残留检测技术发展前景,为检测天然肠衣中兽药残留的进一步发展提供参考。     

动物源性食品中药物多残留分析的研究进展

近年来食品安全检测领域的多残留分析方法在分析通量、成本和适用性方面显示了突出优势。动物源性样品基质复杂、兽药和迁移的农药残留的浓度很低,以多残留方式分析需要发展高效的样品前处理方法和高选择性的检测技术。由于色谱-质谱联用技术在多残留分析中有超过90%的应用,本文综述了近5 a来色谱-质谱检测的动物源性食品的多残留分析。     

液质联用技术在喹诺酮类药物残留中的应用

喹诺酮类药物残留通过生物链在人体内蓄积,进而危害人体健康。因而,需要一种对其含量进行严格控制并且快速准确、高效灵敏的检测技术。液相色谱-质谱联用技术拥有高速高效、高灵敏度、定性分析和定量分析等优势,因而在喹诺酮类药物残留中得到广泛应用。本文简单介绍了喹诺酮类药物残留和液相色谱-质谱联用技术,简析了液质联用技术在喹诺酮类药物残留检测中的应用,期望为检测喹诺酮类药物残留提供参考。     

食品中兽药残留液质联用法检测方法探究

随着科学技术的发展,越来越多的检测技术被投入使用。高效液相色谱-质谱联用仪以液相色谱作为分离系统、质谱作为检测系统,能够快速、高效、准确地分析,并且在稳定性以及挥发性方面占据十分明显的优势,这也是其得到大面积应用的主要原因。在实际针对兽药残留液质进行检测时,可从对动物性食品中受体激素残留的测定、相关技术在操作过程中的注意事项、食品中兽药残留检测的未来这几方面着手。     

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。     

强极性农药残留检测方法的研究进展

草甘膦等强极性农药大量应用于农业中,其本体及代谢物广泛残留于食品、土壤、水质及生态环境中,因其具有一定的毒害性,如何检测备受人们关注。本文对近年来强极性农药残留检测方法的研究进行了总结,包括衍生法-色谱-质谱联用、非衍生法-液相色谱-质谱联用、离子色谱及离子色谱-串联质谱、毛细管电泳法、ICP-MS或ICP-MS/MS与色谱的联用、快速检测技术（酶联免疫吸附法、免疫传感器法、离子迁移谱（IMS）法、分子印迹-化学传感器法、电化学法）等技术的研究现状和应用情况,为强极性农药及其代谢物残留检测提供参考。     

膜萃取技术在食品农药残留分析中的应用

膜萃取是膜分离与液-液萃取相结合的一种新型分离技术.文中综述了在食品农药残留分析中应用较广泛的几种膜萃取技术的装置、原理、特点,分析了影响膜萃取效果的因素.阐述了膜萃取与气相色谱、液相色谱、质谱等仪器的联用技术在食品农药残留分析中的应用,并介绍了一些新型膜萃取技术,讨论了膜萃取技术的发展方向.     

Comprehensive screening of veterinary drugs in honey by ultra-high-performance liquid chromatography coupled to mass spectrometry

In the context of multi-residue screening in honey, a complete methodology was developed for 200 veterinary drugs comprising a sample preparation step and an ultra-high-performance liquid chromatography (UHPLC) coupled to time-of-flight (TOF) mass spectrometry analysis. In addition, specific analytical strategies were developed for two compounds, streptomycin and chloramphenicol, using UHPLC and tandem mass spectrometry (MS/MS). Methodologies were then applied to real honey samples obtained from the Swiss market.     

Mycotoxin analysis: an update

Mycotoxin contamination of cereals and related products used for feed can cause intoxication, especially in farm animals. Therefore, efficient analytical tools for the qualitative and quantitative analysis of toxic fungal metabolites in feed are required. Current methods usually include an extraction step, a clean-up step to reduce or eliminate unwanted co-extracted matrix components and a separation step with suitably specific detection ability. Quantitative methods of analysis for most mycotoxins use immunoaffinity clean-up with high-performance liquid chromatography (HPLC) separation in combination with UV and/or fluorescence detection. Screening of samples contaminated with mycotoxins is frequently performed by thin layer chromatography (TLC), which yields qualitative or semi-quantitative results. Nowadays, enzyme-linked immunosorbent assays (ELISA) are often used for rapid screening. A number of promising methods, such as fluorescence polarization immunoassays, dipsticks, and even newer methods such as biosensors and non-invasive techniques based on infrared spectroscopy, have shown great potential for mycotoxin analysis. Currently, there is a strong trend towards the use of multi-mycotoxin methods for the simultaneous analysis of several of the important Fusarium mycotoxins, which is best achieved by LC-MS/MS (liquid chromatography with tandem mass spectrometry). This review focuses on recent developments in the determination of mycotoxins with a special emphasis on LC-MS/MS and emerging rapid methods.     

Mycotoxin analysis: An update

Mycotoxin contamination of cereals and related products used for feed can cause intoxication, especially in farm animals. Therefore, efficient analytical tools for the qualitative and quantitative analysis of toxic fungal metabolites in feed are required. Current methods usually include an extraction step, a clean-up step to reduce or eliminate unwanted co-extracted matrix components and a separation step with suitably specific detection ability. Quantitative methods of analysis for most mycotoxins use immunoaffinity clean-up with high-performance liquid chromatography (HPLC) separation in combination with UV and/or fluorescence detection. Screening of samples contaminated with mycotoxins is frequently performed by thin layer chromatography (TLC), which yields qualitative or semi-quantitative results. Nowadays, enzyme-linked immunosorbent assays (ELISA) are often used for rapid screening. A number of promising methods, such as fluorescence polarization immunoassays, dipsticks, and even newer methods such as biosensors and non-invasive techniques based on infrared spectroscopy, have shown great potential for mycotoxin analysis. Currently, there is a strong trend towards the use of multi-mycotoxin methods for the simultaneous analysis of several of the important Fusarium mycotoxins, which is best achieved by LC-MS/MS (liquid chromatography with tandem mass spectrometry). This review focuses on recent developments in the determination of mycotoxins with a special emphasis on LC-MS/MS and emerging rapid methods.     

Routine approach to qualitatively screening 300 pesticides and quantification of those frequently detected in fruit and vegetables using liquid chromatography tandem mass spectrometry (LC-MS/MS)

This paper describes an efficient and effective analytical scheme to first screen for 300 pesticides in fruit and vegetables samples using liquid chromatography tandem mass spectrometry (LC-MS/MS) with a commercially enhanced product ion method. Then presumed positive extracts are analysed using a quantitative and confirmatory LC-MS/MS method optimized for 55 pesticides. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) method with acetate buffering (AOAC Official Method 2007.01) was used for sample preparation, which has been previously shown to yield high-quality results for hundreds of pesticide residues in foods. The advantages and disadvantages of both the qualitative screening and quantitative/confirmatory methods and their combination are critically discussed. No false-negatives for the 55 pesticides occurred above 10 ng g^?1 for extracts analysed by both LC-MS/MS methods, and the no false-positives were encountered from the screening analysis (after analyst review) because all presumptive identifications were confirmed in the second analysis. The monitoring scheme was applied during a one-year period on 200 fruit and vegetable samples from Hungarian markets. No pesticide residues were found in half the samples, and twelve violations of European maximum residue limits were detected.     

液相色谱-串联质谱基质效应及其消除方法

综合近年来国内外进行液相色谱-串联质谱方法开发中关于基质效应的相关报道,重点介绍了液相色谱-串联质谱基质效应的消除方法,主要包括:选择合适的样品前处理方法;选择最佳的色谱分离条件;优化的质谱分析参数;使用恰当的内标;采用基质标准溶液校正。这些方法的应用,可有效改善基质效应的影响,优化液相色谱-串联质谱检测方法。     

Determination of aminoglycosides and quinolones in food using tandem mass spectrometry: a review

The widespread use of antibiotics in dairy cattle management may result in the presence of antibiotic residues in food. While rapid screening tests are commonly used to detect the presence of antibiotics in food, more accurate chromatographic-mass spectrometric methods combined with tandem mass spectrometry (MS/MS) are required to determine the identity and quantity of the antibiotic present. These methods (HPLC/MS/MS) may have the greatest potential for accomplishing direct multi-residue identifications in complex biological matrices, such as food. This study reviews recent applications of tandem mass spectrometry in the determination of antibiotic residues, such as aminoglycosides and quinolones in food.     

低温下采用快速液相色谱-质谱联用法分析包装食品中UV油墨光引发剂的迁移

A fast method of liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS) was developed for the analysis of eleven UV ink photoinitiators in packaged food.Chromatographic separation was achieved in a pentafluorophenylpropyl (PFPP) column at 5X2 and acetonitrile:25mM formic acid-ammonium formate(pH 2.7) in gradient elution. To reduce sample treatment,a QuEChERS(quick,easy,cheap,effective,rugged and safe) method for the extraction and clean-up of UV photoinitiators in packaged foods was evaluated.Triple quadrupole working in H-SRM on Ql mode was used for both quantitation and confirmation purposes and the most intense and selective transitions were chosen.Quality parameters of the developed QuEChERS LC-MS/MS method were established and applied for the analysis of photoinitiators in food packaged at ng/kg levels.     

Comparative study of low- versus high-resolution liquid chromatography-mass spectrometric strategies for measuring perfluorinated contaminants in fish

Perfluorinated compounds (PFCs) are usually monitored by high-performance liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) on triple quadrupole instruments. Although not yet widely implemented in the field, high-resolution mass spectrometry (HRMS) today appears as a valuable alternative for these halogenated chemicals due to their significant mass defect. Indeed, this second approach offers a way to cope with particular matrix effects caused by co-eluting and isobaric interferences affecting the measurement of some PFCs in fish. The present study compares three different LC-MS-related instruments and various signal acquisition modes, from low-resolution full-scan and selected ion-monitoring (SIM) mode on a triple quadrupole (QqQ) instrument to high-resolution full-scan or product ion-scan mode on orbital trap (LTQ-Orbitrap) or quadrupole-time-of-flight (Q-TOF) devices. Performances are compared for seven model compounds belonging to seven PFCs subclasses: perfluoralkylsulfonate, perfluoroalkylcarboxylate, perfluoroalkylsulfinate, perfluoroalkyl-sulfonamide, fluorotelomer saturated acid, fluorotelomer unsaturated acid and perfluoroalkylphosphonic acid. Low-resolution MS/MS was found to be unsurprisingly reliable for extended multi-residue monitoring. However, the high stability of PFCs leads to a relatively poor and non-specific fragmentation pathway in MS/MS. In addition, biliary acid-interfering compounds (e.g. taurochenodeoxycholic acid), which where encountered in the present case in fish samples but that may be present in other biological samples, were found particularly disturbing in low-resolution MS/MS. Indeed, these interferences presented the same retention time and diagnostic signals as PFOS, leading to a possible overestimation of the PFOS quantification in LC-MS/MS. On the other hand, high-resolution MS and MS/MS (LTQ-Orbitrap and Q-TOF) provided better results in terms of signal specificity and sensitivity. For instance, the estimated limits of detection (LOD) reached for PFOS on QqQ, Q-TOF and LTQ-Orbitrap instruments were 3.8, 0.7 and 0.5 pg injected, respectively.     

辛辣食物中农药残留检测方法研究- 第1部分: 研究进展

辛辣类食物作为显著味道特色的食物和调味品,普遍为世界各国人们所喜爱。这类作物在种植过程中难免使用农药,其特殊的化学成分会对农药残留检测产生严重干扰。本文对国内外辛辣食物中农药残留检测的净化方法和检测手段进行综述,提取与净化方法主要有固相萃取法、分散固相萃取法、分子印迹固相萃取法、凝胶净化法、微波热处理法、顶空固相微萃取法、搅拌棒萃取法等,分析方法有气相色谱法、气相色谱-质谱法、液相色谱法、液相色谱-质谱法、激光拉曼光谱法等。本文为今后辛辣食物中农药残留分析研究提供参考。     

Determination of fungicide residues in baby food by liquid chromatography-ion trap tandem mass spectrometry

Current European Commission Directives on foods for infants and young children places emphasis on the control of pesticide residues at levels below 10 μg kg(-1). In the present work, a liquid chromatography electrospray ionisation ion trap tandem mass spectrometry (LC-Ion Trap-MS/MS) has been developed for the multiresidue of 10 multiclass fungicides (carbendazim, thiabendazole, imazalil, tridemorph, triadimefon, bitertanol, prochloraz, flutriafol, myclobutanil and diphenylamine) in fruit-based baby food. The developed method is based on a simple sample treatment (QuEChERS), which consists of a liquid-liquid extraction using acetonitrile, followed by a clean-up step based on dispersive solid-phase extraction with primary secondary amine (PSA). Subsequent identification and quantitation was accomplished by liquid chromatography/electrospray tandem mass spectrometry using an ion-trap mass spectrometer in the product ion scan MS/MS mode. Matrix effects were evaluated in LC-MS and LC-MS/MS mode experiments, obtaining a reduction of these effects when working in MS/MS mode for most of the analytes. Limits of detection (LOD) were between 0.5 and 3.0 μg kg(-1) depending on the pesticide studied, all being within European Union regulations for baby food. Finally, the proposed method was applied to 25 baby food samples obtained from local supermarkets. Imazalil, thiabendazole and carbendazim were detected in the studied samples. However, none of the samples tested were found to be upper the EU standard.