分散液液微萃取结合气相色谱-质谱法快速测定葡萄酒中20种农药残留

目的 建立分散液液微萃取结合气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)测定葡萄酒中20种农药残留的分析方法。方法 样品经水稀释后, 采用60 μL氯仿和940 μL乙腈进行分散液液微萃取, 3000 r/min离心5 min, 浓缩后采用气相色谱-质谱联用仪检测。结果 在白葡萄酒与红葡萄酒中进行2.5、5.0、10.0 μg/L的添加回收实验, 本方法的平均回收率为66.7%~126.1%, 相对标准偏差为1.3%~27.2%, 方法的检出限为0.025~0.690 μg/L, 定量限为0.082~2.300 μg/L。结论 本方法前处理过程简单、快速、灵敏度极高、定量结果准确, 适用于葡萄酒中多种农药残留的检测。     

Characterization of rum using solid-phase microextraction with gas chromatography–mass spectrometry

Headspace solid-phase microextraction was used to extract and analyze volatile compounds in different aged rums. The interference of ethanol was resolved with a dilution of the sample at 12% v/v. The extraction procedure, using a 100 μm PDMS fibre with 35 min at 30 °C, permitted the isolation of a large quantity of volatile compounds. One hundred and eighty-four volatile compounds were identified, including 64 esters, 47 benzenic compounds, 16 terpenoids, 14 alcohols, 10 acetals, 9 aldehydes, 6 phenols, 6 ketones, 6 furans, 3 acids and 3 benzopyrans.     

Rice vinegars of different origins: discriminative characteristics based on solid‐phase microextraction and gas chromatography with mass spectrometry,an electronic nose,electronic tongue and sensory evaluation

Eight kinds of commercial rice vinegars from Korea, China and Japan were selected to evaluate their flavour‐related discriminative characteristics based on solid‐phase microextraction and gas chromatography with mass spectrometry (SPME/GC–MS), an electronic nose (e‐nose), electronic tongue (e‐tongue) and subjective sensory evaluation. Principal component analysis patterns based on SPME/GC–MS provided a clear categorical discrimination among the vinegars of three origins. The distribution patterns of the samples were similar between SPME/GC–MS and e‐nose analyses and Korean vinegars were clearly discriminated. A high correlation coefficient was determined between SPME/GC–MS and e‐nose on acetaldehyde (0.948) and diacetyl (0.970). e‐Tongue‐based principal component analysis patterns were subdivided into three regions according to the origin, and Chinese vinegars were clearly discriminated. Sensory panelists recorded origin‐specific scores on flavours for all the samples. In conclusion, SPME/GC–MS, e‐nose and e‐tongue analyses may be useful for discrimination of flavour profiles of rice vinegars of different producer origin. Copyright © 2017 The Institute of Brewing & Distilling     

Free salicylic acid and acetyl salicylic acid content of foods using gas chromatography–mass spectrometry

Dietary salicylates inhibit cycloxygenase-2 and may therefore have anti-inflammatory properties similar to those of aspirin. Individuals that are sensitive to aspirin may also be intolerant to non-acetylated salicylates and could benefit from a low salicylate diet. A total of 76 foodstuffs comprising fruit (16), fresh and prepared vegetables (13), herbs and spices (12), flavourings and sauces (9), beverages (20) and miscellaneous foods (6) were analysed using gas chromatography with mass spectrometric detection and ¹³C carboxyl SA as internal standard. Thirty-seven of the samples contained detectable SA, the highest levels being found in dried herbs (up to 28.6 mg/kg), whereas only one sample (curry sauce) contained detectable ASA at 0.34 mg/kg. Limits of detection for both SA and ASA were matrix-dependent and ranged from 0.008 to 0.23 mg/kg. The results show many inconsistencies with previous data and highlight the need for analysis of a wider range of foods and drinks that are currently available.     

Determination of acrylamide monomer in hydroponically grown tomato fruits by capillary gas chromatography—mass spectrometry

Tomato (Lycopersicon esculentum L) fruits from plants grown hydroponically on polyacrylamide gel were obtained in order to assess any possible uptake of acrylamide monomer from the nutrient solution to the fruit during cultivation. Analysis of acrylamide in the gel itself involved aqueous extraction, bromination and then capillary GC determination with nitrogen-specific detection. By standard addition a level of 0·18 ± 0·01 g kg^?1 residual monomer was found to be present in a sample of gel used by an experimental horticultural station. Tomato fruits were analysed by extraction of the aqueous phase, bromination, silica-gel cartridge clean-up and capillary GC–MS determination by selected ion monitoring. The recovery of the method was 26–62% but losses throughout were compensated for by use of 2,3-dibromo-2-dimethylpropionamide internal standard. No acrylamide monomer could be detected in tomato fruits from plants grown hydroponically on polyacrylamide gel at a limit of detection of 1 × 10^?6 g kg^?1, demonstrating that the monomer is not transferred from the growing medium into tomato fruits.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

气相色谱-质谱联用法和高效液相色谱法测定4种人参酒中的皂苷和挥发性成分

目的 探究4种人参酒中皂苷和挥发性成分的差异.方法 将4种参粉碎后用乙醇浸泡后,经顶空固相微萃取结合气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)测定其挥发性成分,再用高效液相色谱法(high performance liquid chromatograph...     

Multiresidue method for the determination of 77 pesticides in wine using QuEChERS sample preparation and gas chromatography with mass spectrometry

A method based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) sample preparation method and gas chromatography with mass spectrometric detection by selected ion monitoring (GC/MS-SIM) was developed for simultaneous determination of 77 pesticide residues in wine. An extraction of 10 ml of sample with acetonitrile followed by liquid–liquid partition formed by the addition of 4 g MgSO₄ and 3 g NaCl was applied in the sample preparation. The clean-up was carried out by applying dispersive solid-phase with 150 mg MgSO₄ as well as 50 mg primary secondary amine (PSA). One quantitation ion and at least two identification ions were selected in the analytical method for each pesticide compound by GC/MS. The recovery data were obtained by spiking blank samples at two concentration levels (0.05 and 0.2 mg l^?1). The recoveries of all pesticides were in the range 70–110%, with intra-day precision of less than 15%, and the inter-day precision of less than 22% and 15% for 0.05 and 0.2 mg l^?1 fortification levels, respectively. Linearity was between 0.02 and 2 mg l^?1 with determination coefficients (R ²) greater than 0.98 for all compounds. The limits of quantification (LOQs) for the 77 pesticides ranged from 0.003 to 0.05 mg l^?1. This method was applied for routine analysis in market products.     

Rapid determination of ethyl carbamate in Chinese rice wine using headspace solid‐phase microextraction and gas chromatography–mass spectrometry

Ethyl carbamate (EC) is a naturally occurring toxic contaminant that may imply a risk to human health and is usually found in alcoholic beverages such as Chinese rice wine. An automated procedure for the rapid determination of EC in Chinese rice wine was developed by headspace solid‐phase microextraction (HS‐SPME) coupled to gas chromatography–mass spectrometry (GC‐MS). Using propyl carbamate as internal standard, the optimized HS‐SPME sampling with a polyacrylic fibre was 45 min at 70°C after applying 38.8% NaCl to saturate the sample. This method showed good linearity over a range of 25–600 µg L^?1 (R² = 0.997). The recovery, relative standard deviation and limit of detection were 90.21–97.35%, lower than 2.89% and 1.19 µg L^?1, respectively. Additionally, the ethanol concentration had no effect on the analysis of EC. The total analysis time of 57 min per sample in continuous determination was twice as fast as the widely used solid‐phase extraction–GC‐MS method. This solvent‐free HS‐SPME‐GC‐MS procedure is suitable for the rapid, automated, and therefore convenient, determination of EC in Chinese rice wine. Copyright © 2012 The Institute of Brewing & Distilling     

QuEChERS前处理结合高效液相色谱法及高效液相色谱-串联质谱法检测葡萄酒中3种赭曲霉毒素

目的建立QuEChERS净化技术结合高效液相色谱法及高效液相色谱-串联质谱法检测葡萄酒中赭曲霉毒素A(OTA)、赭曲霉毒素B(OTB)和赭曲霉毒素C(OTC)3种赭曲霉毒素的方法。方法对QuEChERS净化条件和高效液相色谱及高效液相色谱-串联质谱检测条件进行优化,葡萄酒样品先用乙腈-冰乙酸(90∶10,V/V)进行酸化稀释,离心后取上清液经C_(18)+SiO_2+MgSO_4净化剂组合净化过滤,待测样液经液相色谱C_(18)柱(4.6 mm×250 mm,5μm)梯度洗脱分离后,分别采用荧光检测器和串联质谱电喷雾技术,在多反应监测(MRM)模式下,实现同时对葡萄酒中OTA、OTB和OTC三种赭曲霉毒素的定性和定量分析。结果方法最低定量限(LOQ)均为2.0μg/kg,相对标准偏差(RSD)为2.01%～7.52%(n=6)。结论该方法操作方便、灵敏度高、重现性好,适用于日常监管工作中对葡萄酒中赭曲霉毒素的检测。