Comparison of headspace-SPME-GC–MS and LC–MS for the detection and quantification of coumarin,vanillin, and ethyl vanillin in vanilla extract products

A headspace-solid phase micro-extraction (HS-SPME) GC–MS method has been developed for the determination of coumarin, vanillin and ethyl vanillin in vanilla products. Limits of detection ranged from 1.33 to 13.2 ng mL⁻¹. Accuracy and precision data for the method were measured and compared to those obtained using LC-ESI-MS. A survey of 24 commercially available vanilla products was completed using both techniques. No coumarin was detected in any of the samples. Examination of the GC–MS chromatograms revealed the presence of 18 other flavor related compounds in the samples. The method validation and sample analysis data using HS-SPME-GC–MS were comparable to those obtained using the LC–MS method. Because the two methods are conceptually different from one another, both methods would not be subject to the same interferences. This would allow them to be used as confirmatory methods for each other.     

Application of an HPLC–MS/MS method for mycotoxin analysis in commercial baby foods

This article describes the validation of an analytical method for the detection of 21 mycotoxins in baby food. The analytical method is based on the simultaneous extraction of selected mycotoxins by matrix solid-phase dispersion (MSPD) followed by liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) using a hybrid triple quadrupole-linear ion trap mass spectrometer (QTRAP®). Information Dependent Acquisition (IDA), an extra confirmation tool for samples that contain the selected mycotoxins, was used. The matrix effects were evaluated, and the corrections for the matrix effects were performed using two calibration approaches: external matrix-matched calibration and internal standard calibration. Matrix-matched calibration was ultimately used for accurate quantification, and the recoveries obtained were generally higher than 70%. The analytical method was applied to the analysis of 35 samples of commercial baby foods. No sample exceeded the maximum limit (ML) fixed by the European Union for these mycotoxins in baby food. However, this survey highlighted the occurrence of mycotoxins in cereal-based infant foods.     

A rapid LC/MS/MS method for the analysis of nonvolatile antiinflammatory agents from Mentha spp

Abstract: Mints (Mentha spp.), aromatic crops grown largely for their essential oils, also are rich sources of nonvolatile antiinflammatory agents. Identification and quantitation of the constituents responsible for their antiinflammatory activity is challenging owing to the lack of suitable chromatographic methodology. In the present research, the simultaneous quantitation of antiinflammatory constituents rosmarinic acid, oleanolic acid, and ursolic acid in mints was attained by using a unique tandem HPLC column system coupled with an electrospray ionization mass detection (MRM mode). The ion mode optimization for rosmarinic acid under negative and triterpenoid acids under positive was achieved by setting 2 time segments in a single run where the polarity mode was switched from negative (0 to 10 min) to positive (10 to 40 min). For the investigated concentration ranges of antiinflammatory agents in mints, good linearities (r²≥ 0.998) were obtained for each calibration curve. Validation of precision and accuracy for this method showed that intra‐ and inter‐day repeatabilities for all analytes were less than 5.51%, and the recoveries varied from 97.8% to 99.3%. The developed LC/MS/MS assay provides a suitable quality control method for the determination of antiinflammatory constituents in Mentha spp. There is a wide range of diversity in the natural product composition for these acids across the Mentha germplasm collection evaluated. The presence of these antiinflammatory acids in post‐distilled mints shows that value‐added nutraceutical enriched products can be developed with proper processing and recovery systems in addition to the distillation and capture of the valuable volatile essential oils. Practical Application: Results from this research would benefit both commercial farmers growing mint for essential oil and those in the food industry where value‐added phytopharmaceutical enriched products can be developed with proper processing, quality control, and recovery systems during mint essential oil distillation.     

Development of an accelerated solvent extraction,ultrasonic derivatisation LC‐MS/MS method for the determination of the marker residues of nitrofurans in freshwater fish

A rapid method using accelerated solvent extraction (ASE) and ultrasound enhanced derivatisation has been developed for the quantitative determination of metabolites of nitrofurans, namely 3‐amino‐2‐oxalidinone (AOZ), 5‐morpholinomethyl‐3‐amino‐2‐oxalidinone (AMOZ), 1‐amino‐hydantoin (AHD) and semicarbazide (SEM), in muscle and skin of carp and finless eel. The target analytes were extracted using ASE, ultrasonic derivatisation for 1?h and then purified by solid phase extraction. Averaged decision limits (CCα) and detection capability (CCβ) of the method were in the range of 0.07–0.13 and 0.31–0.49?µg?kg^?1 in carp and finless eel, respectively. The accuracy in terms of recovery was in the range 77.2–97.4%. The simplified and traditional methods were compared with incurred residue samples. The simplified method reduced the derivatisation time and has been applied to the determination of nitrofurans residues in fish.     

Quantitative analysis of 3-alkyl-2-methoxypyrazines in German Sauvignon blanc wines by MDGC–MS or MDGC–MS/MS for viticultural and enological studies

A method for trace-level analysis of 3-alkyl-2-methoxypyrazines (MPs) based on mixed-bed cation-exchange solid phase extraction followed by heart-cut multidimensional gas chromatographic analysis was applied in a trial on viticultural and enological treatments of Sauvignon blanc wines produced in Germany. The quantification was based on a stable isotope dilution assay using deuterated MPs. For method comparison, detection was either with selected ion monitoring with a quadrupole mass spectrometer (MS) or after selected reaction monitoring using a triple quadrupole MS. Comparable performance for MP detection in the lower ng L^?1 concentration range was found for both detection methods; however, in some cases, matrix problems could only be solved with MS/MS detection. It could be shown that MP levels varied considerably between the investigated vintages, with concentrations often well below 10 ng L^?1. Leaf removal as a viticultural trial was a measure to decrease MP concentrations; however, the effects observed were low in the vintages studied here. Cold maceration and stem addition to the must were found as valuable enological means for increasing the MP concentration and improving the green sensory notes typical for cold climate Sauvignon blanc wines.     

Finding of pesticides in fashionable fruit juices by LC–MS/MS and GC–MS/MS

Products labelled as containing extracts from two mushrooms (cordyceps plus reishi) and the juices from açaí, goji, mangosteen, noni, pomegranate, and sea buckthorn have been analysed for 174 different pesticides, using the validated QuEChERS method for sample preparation and electrospray LC–MS/MS in the positive ion mode for analysis. Pesticides were found in 10 of the 21 samples analysed. Most pesticides found were below the tolerance levels (1–6 μg/g, depending on the pesticide), but some were not. This included boscalid, dimethomorph, iprovalicarb, pyridaben, pyrimethanil, and imazalil, for which there is no tolerance reported or zero tolerance in any fruit. However, genuine açaí that was harvested in the state of Pará and lyophilised in Rio de Janeiro had no detectable pesticides, when analysed by both LC–MS/MS and GC–MS/MS, which can detect 213 more pesticides and industrial chemicals. Likewise no pesticides were found in one sample each of cordyceps plus reishi, sea buckthorn and noni.     

Application of GC–MSD and LC–MS/MS for the determination of priority pesticides in baby foods in Serbian market

Babies and small children are especially sensitive population to the exposure to environmental contaminants. Their small mass and developing systems, including brain development may show adverse health effects from even low levels of contamination on a chronic or single dose case. In this paper one extraction method and two chromatographic techniques for the determination of pesticide residues in baby food were evaluated. A liquid chromatography–tandem mass spectrometry technique combined with electrospray ionization (ESI), (LC–MS/MS) and gas chromatography–mass spectrometry detection (GC–MSD) technique were applied in the detection of 50 pesticides in baby food. So-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method was used as a sample preparation procedure. The recoveries were investigated at three levels (5, 10 and 50 μg/kg) and the results obtained showed compliance with the contemporary EU requirements with a few exceptions. LOQs for most of the tested pesticides were below the EU MRLs (10 μg/kg), except deltamethrin, cypermethrin, fenvalerate, phosalone and beta-cyfluthrin (LOQs were 10 μg/kg). Both techniques were applied in the analysis of 50 samples of baby food manufactured in Serbia.     

LC/MS/MS法分析食品中的三聚氰胺

奶粉类食品前处理1.所需试剂及耗材1%三氯乙酸溶液,0.1mol/L盐酸溶液,5%氨水-甲醇溶液,以及OasisMCX固相萃取柱(60mg/3mL,或相当者),使用前分别用3mL甲醇、3mL0.1mol/L盐酸溶液对固相萃取柱进行预处理,并保持柱体的湿润。     

Analytical strategy for the determination of non-steroidal anti-inflammatory drugs in plasma and improved analytical strategy for the determination of authorised and non-authorised non-steroidal anti-inflammatory drugs in milk by LC–MS/MS

A sensitive and selective method for the determination of six non-steroidal anti-inflammatory drugs (NSAIDs) in bovine plasma was developed. An improved method for the determination of authorised and non-authorised residues of 10 non-steroidal anti-inflammatory drugs in milk was developed. Analytes were separated and acquired by high performance liquid chromatography coupled with an electrospray ionisation tandem mass spectrometer (ESI–MS/MS). Target compounds were acidified in plasma, and plasma and milk samples were extracted with acetonitrile and both extracts were purified on an improved solid phase extraction procedure utilising Evolute? ABN cartridges. The accuracy of the methods for milk and plasma was between 73 and 109%. The precision of the method for authorised and non-authorised NSAIDs in milk and plasma expressed as % RSD, for the within lab reproducibility was less than 16%. The % RSD for authorised NSAIDs at their associated MRL(s) in milk was less than 10% for meloxicam, flunixin and tolfenamic acid and was less than 25% for hydroxy flunixin. The methods were validated according to Commission Decision 2002 European Commission Decision. 2002. Decision(2002/657/EC) of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and interpretation of results. Off J Eur Commun, L221: 8–36.  [Google Scholar]/657/EC.     

Pesticide Residue Rapid Extraction from Ginseng Tea Using a Modified Luke Method for GC–MS

A modified Luke rapid detection method followed by gas chromatography–mass spectrometry (GC–MS) has been developed for the simultaneous determination of 42 pesticides in ginseng tea. This method uses acetone and n-hexane solution to extract and partition pesticides. Ginseng tea samples were mixed with acetone, water and n-hexane solution, and then partitioned by vortex. After the partition, the top layer (n-hexane) was transferred into a centrifuge tube containing primary secondary amine (PSA), graphitized carbon black (GCB) and C₁₈ for purification. And then the centrifuge supernatant was injected into GC–MS. The Luke method was applied in ginseng tea sample detection, and we confirmed that this method can easily extract various types of pesticides from ginseng tea samples. The rates of recovery for pesticides studied were satisfactory, ranging from 65.5 to 109.0 % with a relative standard deviation (RSD) of less than 12 %. The limits of quantification (LOQs) ranged between 0.5 and 11.5 μg·kg^?1. The modified Luke method is quick and easy.     

SPME followed by GC–MS: a powerful technique for qualitative analysis of honey volatiles

Volatile compounds from 40 honey samples of different botanic origin were analyzed by SPME followed by GC–MS. In order to obtain complementary data for an overall characterization of honey aroma, two different SPME fiber coatings (polyacrylate and carboxen/polydimethylsiloxane) were employed. The use of both fibers with a single chromatographic column afforded the identification or characterization, based on GC retention and mass spectral data, of a total of 193 volatile components. A total of 166 honey volatiles were characterized (146 identified) from CAR/PDMS data, this fiber being the most appropriate for isolation of low molecular weight compounds. Polyacrylate fiber was better for extraction of polar semivolatiles, allowing to identify 120 compounds and to characterize 132. Besides typical nectar components such as limonene, linalool, etc., different compounds from fermentation (ethanol and 2,3-butanediol), processing (furan derivatives), hive treatment (thymol), etc. were detected. Although many volatiles were common to most honey samples analyzed, other seemed to be characteristic of certain honey types. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Is there any place for alimentary probiotics, prebiotics or synbiotics, for patients with inflammatory bowel disease?

The pathogenesis of inflammatory bowel disease (IBD) involves an interaction between genetically determined host susceptibility, dysregulated immune response, and the enteric microbiota. Ecological treatments including probiotics, prebiotics, and synbiotics are actively studied in Crohn's disease (CD), ulcerative colitis (UC) and pouchitis. We review herein the literature on the rational use of probiotics in IBD considering efficacy (as evaluated in randomized controlled trials), mechanisms of action and safety issues. A probiotic effect is strictly restricted to one defined strain and cannot be generalized from one to another. There is evidence of efficacy of some probiotic drugs in pouchitis (VSL#3), and in the prevention of recurrence of UC (Escherichia coli Nissle 1917). However, the evidence for efficacy of probiotic drugs in CD is still low as well as that of dietary ecological treatments. Despite an ecological (hopefully nutritional) treatment of IBD is promising, many questions remain unanswered and further clinical and fundamental studies are needed.     

HPLC-DAD和LC/MS/MS测定豆奶中三聚氰胺

目的:建立二极管阵列高效液相色谱仪和三重四级杆液质联用仪对豆奶中三聚氰胺的测定方法。方法:采用三氯乙酸和乙腈为提取剂、蛋白质为沉淀剂,提取液过净化柱纯化。结果:三重四级杆液质联用法对三聚氰胺的检出限为0.001 5 mg/kg,标准曲线在0.01~0.5μg/mL范围内,R~2为0.999 8,线性良好,再回收率为85%~89%,适用于检测低浓度的样品;二极管阵列高效液相色谱法检出限为0.024 mg/kg,标准曲线在0.5~100μg/mL范围内,R~2为0.999 9,线性良好,回收率为83%~91%,可以快速地对高浓度样品进行筛查。结论:以上两种检测方法结合使用,可检测0.01~100 mg/kg的三聚氰胺含量,极大地拓宽了检测范围。     

基于UPLC/Q-TOF MS/MS的花生油成分分析

采用超高效液相色谱-串联四级杆飞行时间质谱(UPLC/Q-TOF MS/MS)联用仪对花生油甲醇提取液分离检测,分析花生油成分,并通过二级质谱图和标准品确定物质。结果表明:正离子模式下检出86种化合物,鉴定30种物质,其中芥酸、棕榈酰胺、硬酯酰胺、油酸酰胺、11Z-二十二碳二烯酸为已知的花生油成分,亚油酰乙醇胺、亚油酰胺、鞘氨醇、N-油酰乙醇胺、十八碳四烯酸、顺-4-癸二酸等26种物质均为首次被检出;在负离子模式下,共检出27种化合物,鉴定15种物质,其中包括花生油中常见的7种脂肪酸,首次检出(Z)-13-氧-9-十八烯酸、蓖麻油酸、烯油酸、13-羟基十八酸和2(R)-羟基海藻酸5种脂肪酸和其他3种物质。     

基于UPLC/Q-TOF MS/MS的芝麻油成分分析

为发现芝麻油中新成分,通过UPLC/Q-TOF MS/MS对4种芝麻油甲醇提取液进行检测分析。结果表明：4种芝麻油中共发现143种共同物质,其中正离子模式71种,负离子模式72种。共同物质中鉴定出77种物质,其余66种为未鉴定成分;77种鉴定成分中包括脂肪酸及衍生物(8种)、芝麻素、芝麻林素、硬脂酰胺等12种已知成分,其余65种为新发现成分;新发现成分包括油酸酰胺、棕榈酰胺、亚油酰胺、芥酸酰胺、8-甲基-N-香草基壬酰胺、辣椒酰胺、N-硬脂酰丙氨酸等17种脂肪酸酰胺,十六碳烯酸、十八碳烯酸等22种脂肪酸及衍生物,5-脱氧基维醇、天孢菌素等5种类黄酮,马泰树脂醇、银杏酸等21种其他成分。芝麻油中含有大量新成分和未知成分,富含的脂肪酸、脂肪酸酰胺、类黄酮、木脂素等物质可解释其独特生理功能。     

MS发布高速印花机

近日，意大利MS公司发布了高速数码印花机LaRio。该机生产速度可达每分钟75m，幅宽1．8m，可完成8000m＾2／h印花业务，每天产能接近20万m＾2，堪比传统圆网印花机。该机目前已有一台在意大利投入实际生产使用。该机采用非接触的喷墨打印技术，实现对于墨水（染料）的精微控制，无须制版，印花得色率高，     

MS—1型白瓜籽脱壳机上料,排序装置性能研究

本文就上料，排序装置的带速，白瓜籽规格，平面上倾角对上籽率，工位单籽承的影响进行实验研究。     

Tandem solid phase extraction coupled to LC–ESI–MS/MS for the accurate simultaneous determination of five heterocyclic aromatic amines in processed meat products

Carcinogenic heterocyclic aromatic amines are difficult to measure since only trace levels are present in processed meat products. In this study, typical heterocyclic aromatic amines, including 2-amino-3-methylimidazo [4,5-f] quinoline (IQ), 2-amino-3,4-dimethylimidazo [4,5-f] quinoline (MeIQ), 2-amino-3,8-dimethyli-midazo [4,5-f] quinoxaline (MeIQx), 2-amino-3,4,8-trimethylimi-dazo [4,5-f] quinoxaline (4,8-DiMeIQx), 2-amino-1-methyl-6-ph-enylimidazo [4,5-b]pyridine (PhIP), were studied to develop a sensitive and accurate method for their rapid quantification in animal-derived products, with 2-Amino-3,4,7,8-dimethylimidazo [4,5-f] quinoxalline (TriMeIQx) as an internal standard. Liquid chromatography–electrospray-tandem mass spectrometry conditions were analyzed to enhance detection sensitivity. Diatomaceous earth was employed to extract heterocyclic aromatic amines from meat samples, and the analytes were purified and enriched using tandem solid phase extraction, with siliprep propylsulfonic acid coupled to a C₁₈ cartridge. A number of parameters, including pH, eluent and volume, were carefully optimized to improve the extraction and purification efficiency. Under the optimal experimental conditions, the limits of detection for each analyte within the meat matrix were 0.5 pg (injected). The established method was applied to evaluate commercial meat products. At three spiked levels of 0.2, 1 and 4 μg kg⁻¹, the recoveries and relative standard deviations were measured as 76.4–122.2 and 0.9–23.4%, respectively, suggesting the developed method is promising for the accurate quantification of heterocyclic aromatic amines at trace levels in processed meats.     

Omega-6 for Body, Omega-3 for Brain: Balance for Brain Development in Children (英文原文)(Online First, Recommended Article)

Food must supply a balance of nutrients to support both brain and body. The human brain makes us uniquely human. Essential fatty acids are part of the metabolic pathways that define tissue structure and function. Omega-6 (O6) linoleic acid (LA6) has long been known to be required for skin structure, and as a precursor for inflammatory, thrombotic, immune, and other signaling molecules. Omega-3 (O3) alpha-linolenic acid (ALA3) and particularly its long chain product docosahexaenoic acid (DHA3) has a key structural role in the brain, retina, and related neural tissue. In the 20th century western world, inexpensive, high quality oils primarily from LA6-rich/O3-poor vegetable seed oils became dominant fats produced by the food industry. Provision of LA6-rich/O3-poor oils as the sole source of fat in the diets of pregnant animals causes O3 deficiency and poor brain development, primarily because high LA6 antagonizes metabolism of all O3, creating an artificial metabolic demand for O3. Data developed over the last 2~3 decades show that provision of low LA6 combined with preformed DHA3 optimizes brain function. Recent studies emphasize the importance of nutrition to support brain development, with newer findings showing particular importance of fatty acid balance in malnourished children. The World Health Organization (WHO) through the Codex Alimentarius (“Code for Food”) is increasingly recognizing the primacy of brain health and in part on that basis recently acted to recommend balanced fat for Ready-to-Use-Therapeutic Foods used to treat children with severe acute malnutrition. Similar principles are likely to be important in older persons. Industry now has the tools to adjust the composition of oils to support brain health throughout the life cycle.