Quantitation of Mycotoxins in Food and Feed from Burkina Faso and Mozambique Using a Modern LC-MS/MS Multitoxin Method

In this study an LC-MS/MS multitoxin method covering a total of 247 fungal and bacterial metabolites was applied to the analysis of different foods and feedstuffs from Burkina Faso and Mozambique. Overall, 63 metabolites were determined in 122 samples of mainly maize and groundnuts and a few samples of sorghum, millet, rice, wheat, soy, dried fruits, other processed foods and animal feeds. Aflatoxin B(1) was observed more frequently in maize (Burkina Faso, 50% incidence, median = 23.6 μg/kg; Mozambique, 46% incidence, median = 69.9 μg/kg) than in groundnuts (Burkina Faso, 22% incidence, median = 10.5 μg/kg; Mozambique, 14% incidence, median = 3.4 μg/kg). Fumonisin B(1) concentrations in maize were higher in Mozambique (92% incidence, median = 869 μg/kg) than in Burkina Faso (81% incidence, median = 269 μg/kg). In addition, ochratoxin A, zearalenone, deoxynivalenol, nivalenol, and other less reported mycotoxins such as citrinin, alternariol, cyclopiazonic acid, sterigmatocystin, moniliformin, beauvericin, and enniatins were detected. Up to 28 toxic fungal metabolites were quantitated in a single sample, emphasizing the great variety of mycotoxin coexposure. Most mycotoxins have not been reported before in either country.     

环境内分泌干扰物辛基酚、壬基酚及短链壬基酚聚氧乙烯醚残留同步检测方法

建立了环境内分泌干扰物辛基酚、壬基酚及短链壬基酚聚氧乙烯醚降解产物的高效液相色谱串联质谱分析方法。选择易受环境污染的玉米、白菜等农产品及目标物可能迁移到环境中的食品包装材料为研究对象,经过液液萃取、浓缩,乙腈甲苯（3：1）溶液溶解,经ENVITMCarblI／PSA氨基固相萃取柱净化,甲醇一二氯甲烷（4：3）溶液为洗脱液。采用Agilent ZORBAX RX-C18柱,以甲醇：10mmol·L^-1乙酸铵（9：1）为流动相,梯度洗脱分离后,在LC—MS／MS多反应监测模式下正负离子同时扫描进行定性与定量分析。结果表明,该方法对辛基酚、壬基酚、壬基酚一氧乙烯醚和壬基酚二氧乙烯醚的检出限分别为O．03、0.6、1．6、0．03μg·kg^-1,在不同基质中添加浓度为0．5-5μg·kg^-1的四种物质平均回收率在62％～113％之间。对实际样品进行检测时,在蔬菜和粮食作物及其包装材料中分别检测到不同含量的上述物质,表明该方法准确、快速、灵敏度高,可用于农产品和食品包装材料中该类物质的监控。     

A validated multianalyte LC-MS/MS method for quantification of 25 mycotoxins in cassava flour, peanut cake and maize samples

This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of 25 mycotoxins in cassava flour, peanut cake and maize samples with particular focus on the optimization of the sample preparation protocol and method validation. All 25 mycotoxins were extracted in a single step with a mixture of methanol/ethyl acetate/water (70:20:10, v/v/v). The method limits of quantification (LOQ) varied from 0.3 μg/kg to 106 μg/kg. Good precision and linearity were observed for most of the mycotoxins. The method was applied for the analysis of naturally contaminated peanut cake, cassava flour and maize samples from the Republic of Benin. All samples analyzed (fifteen peanut cakes, four maize flour and four cassava flour samples) tested positive for one or more mycotoxins. Aflatoxins (total aflatoxins; 10-346 μg/kg) and ochratoxin A (相似文献   

Simultaneous determination of chloramphenicol and aflatoxin M1 residues in milk by triple quadrupole liquid chromatography-tandem mass spectrometry

A reliable, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of chloramphenicol and aflatoxin M(1) in milk has been developed. This method includes simple extraction of sample with acetonitrile, separation on a MGIII-C(18) column using 5 mM ammonium acetate aqueous solution/methanol (60:40, v/v) as mobile phase, and MS/MS detection using multiple reaction monitoring mode. The method was validated according to Commission Decision 2002/657/EC. The limits of detection (LODs) were 0.05 μg/kg for chloramphenicol and 0.005 μg/kg for aflatoxin M(1.) The limits of quantification (LOQs) were 0.2 μg/kg for chloramphenicol and 0.02 μg/kg for aflatoxin M(1). The recovery values ranged from 88.8% to 100.6%, with relative standard deviation lower than 15% in all cases, when samples were fortified at three different concentrations. The decision limits (CCα) and detection capability (CCβ) of the method were also reported. This method has been successfully applied for simultaneous analysis of chloramphenicol and aflatoxin M(1) residues in milk from local supermarkets in China.     

Simultaneous determination of five plant growth regulators in fruits by modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and liquid chromatography-tandem mass spectrometry

An effective method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and optimized to obtain a complete separation of five representative plant growth regulators (PGRs) [gibberellic acid, 2,4-dichlorophenoxyacetic acid (2,4-D), thidiazuron, forchlorfenuron, and paclobutrazol] in fruits. Extraction was performed with acetonitrile containing 0.1% (v/v) acetic acid, applying modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) methodology. LC-MS/MS conditions including composition of mobile phases and mass spectrometry (MS) conditions were evaluated to achieve the highest sensitivity in MS detection. All of the data acquisition was employed in the segmented multiple-reaction monitoring mode for the selected negative and positive transition ions. The octadecylsilyl (C18) dispersive solid-phase extraction (SPE) sorbent was found to provide the more satisfied recoveries than primary secondary amine (PSA) and graphitized carbon black (GCB) for five target PGRs. The optimized method allowed for recoveries of 76-112% for the five PGRs from fruit samples with relative standard deviation (RSD) values less than 10%. Limits of quantification (0.5-16.5 μg/kg) were lower than the maximum limit of residues established for PGRs. The results demonstrated that the developed LC-MS/MS and QuEChERS extraction method is highly effective for analyzing trace amounts of target PGRs in fruit samples. Finally, the method was successfully used to detect residual PGRs in Beijing, China, in 2010. The concentrations of 2,4-D (5.1-1503 μg/kg) and paclobutrazol (1-1381 μg/kg) found in orange and peach, respectively, suggesting that the use of these PGRs in these fruits should be regulated in China in the future.     

Simultaneous determination of four biogenic and three volatile amines in anchovy by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry

A new method has been developed and validated for the simultaneous determination of four biogenic (putrescine, cadaverine, histamine, and tyramine) and three volatile amines (trimethylamine, triethylamine, and tripropylamine) in anchovy. Separation and determination of the selected compounds were carried out by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS), using an electrospray ionization source (ESI) in positive ion mode. Chromatographic separation was carried out using an aqueous solution of formic acid (0.1%) and methanol as mobile phase in gradient mode. The method was validated, and mean recoveries were evaluated at three concentration levels (75, 150, and 250 μg/kg), ranging from 70 to 110% at the three levels assayed. Intra- and interday precision, expressed as relative standard deviation (RSD), were lower than 15% and 20%, respectively. Limits of quantitation (LOQs) were 25 μg/kg for all cases, except for that of TMA, which was set at 60 μg/kg. The developed procedure was applied to determine the target compounds in anchovy samples stored during 7 days at 4 °C, observing the increasing in the concentration of these compounds at longer storage time.     

Development of a method for the simultaneous determination of six sulfonylurea herbicides in wheat, rice, and corn by liquid chromatography-tandem mass spectrometry

A sensitive and reliable method was developed and validated for trace determination of sulfonylurea herbicides residues in cereals (wheat, rice, and corn) by liquid chromatography-tandem mass spectrometry. The selected analytes were ethoxysulfuron, ethametsulfuron-methyl, bensulfuron-methyl, chlorimuron-ethyl, pyrazosulfuron-ethyl, and cyclosulfamuron. In this work, the extraction procedure was performed by using a mixture solvent of phosphate buffer (pH 9.5)/acetonitrile (8:2, v/v) as the extraction solvent and then was cleaned up by using Spe-ed C18/18% SPE cartridges, providing good recoveries for all of the tested analytes and with no matrix effects affecting method accuracy. The limits of detection for the studied analytes in cereal samples were between 0.043 and 0.23 μg kg(-1), and the limits of quantification were between 0.14 and 0.77 μg kg(-1), lower in all cases than the maximum residue limits permitted by the European Union for this kind of food. The developed methodology has demonstrated its suitability for the monitoring of these residues in cereal samples with high sensitivity, precision, and satisfactory recoveries.     

Development of multiresidue analysis for twenty phthalate esters in edible vegetable oils by microwave-assisted extraction-gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry

A novel multiresidue analysis method is developed for the determination of twenty phthalate esters at the μg/kg level in edible vegetable oils by microwave-assisted extraction-gel permeation chromatography-solid phase extraction-high resolution gas chromatography-tandem mass spectrometry (MAE-GPC-SPE-HRGC-MS/MS). The samples were extracted with methanol under microwave incubation. Cleanup was carried out with GPC followed by a further C18 SPE column and then separated by the HP-5MS capillary column under a temperature program. The eluents were qualitatively and quantitatively determined by tandem mass analyzer with selected reaction monitoring (SRM) type and positive ion mode. The calibration curves showed good linearity in the range 5 μg/kg to 2.50 mg/kg with correlation coefficients larger than 0.999. Low detection limits (LODs) of 0.218-1.367 μg/kg and quantification limits (LOQ) of 0.72-4.51 μg/kg were achieved. The mean recoveries were in the range from 93.04% to 104.6% at 5, 15, and 40 μg/kg spiked levels, and the relative standard deviations (RSDs) were in the range of 1.01% and 5.26% (n = 7). This method could potentially overcome the interference from large amounts of lipids and pigment. The real sample test showed this method can be used for sensitive and accurate determination and confirmation of phthalate ester residues in high-fat and complex samples.     

Determination of pesticides and PCBs in virgin olive oil by multicolumn solid-phase extraction cleanup followed by GC-NPD/ECD and confirmation by ion-trap GC-MS

A multicolumn solid-phase extraction cleanup for the determination of organophosphorus (OP) and organochlorine (OC) pesticides plus PCB congeners in virgin olive oil is presented. The method involves dissolution of the olive oil in hexane, followed by a cleanup system using a diatomaceous earth column (Extrelut-QE) with reversed (C(18)) and normal (alumina) phase SPE columns. Determination of OPs was by GC-NPD, while the OCs and PCBs were analyzed using GC-ECD. Recovery assays for OPs varied from 81.7% to 105.3%, for OCs ranged between 74.3% and 99.4%, while for PCBs were from 60.1% to 119.2%. Quantitation limits ranged from 10 to 25 microg/kg olive oil for OPs, and from 1 to 6 microg/kg olive oil for OCs and PCBs. In the case of positive samples, the confirmation of pesticide identity was performed by ion-trap GC-MS/MS. The applicability of the method was assayed with 19 virgin olive oil samples collected from different olive mills of Aragón (Spain). Only one OP pesticide (acephate) was detected in one sample at a concentration of 10 microg/kg. Organochlorine pesticides were found in 5-47% of samples at very low levels ranging from 1.5 to 5.2 microg/kg. PCBs were found in 20-90% of samples, showing concentrations between 2.3 and 17.3 microg/kg.     

Development of a solid-phase extraction coupling chemiluminescent enzyme immunoassay for determination of organophosphorus pesticides in environmental water samples

Solid-phase extraction (SPE) and direct competitive chemiluminescence enzyme immunoassay (dcCL-EIA) were combined for the detection of organophosphorus pesticides (OPs) in environmental water samples. dcCL-EIA based on horseradish peroxidase labeled with a broad-specificity monoclonal antibody against OPs was developed, and the effects of several physicochemical parameters on dcCL-EIA performance were studied. SPE was used for the pretreatment of water samples to remove interfering substances and to concentrate the OP analytes. The coupling of SPE and dcCL-EIA can detect seven OPs (parathion, coumaphos, phoxim, quinalphos, triazophos, dichlofenthion, and azinphos-ethyl) with the limit of quantitation below 0.1 ng/mL. The recoveries of OPs from spiked water samples ranged from 62.5% to 131.7% by SPE-dcCL-EIA and 69.5% to 112.3% by SPE-HPLC-MS/MS. The screening of OP residues in real-world environmental water samples by the developed SPE-dcCL-EIA and their confirmatory analysis using SPE-HPLC-MS/MS demonstrated that the assay is ideally suited as a monitoring method for OP residues prior to chromatographic analysis.     

Levels of bisphenol A in canned liquid infant formula products in Canada and dietary intake estimates

A sensitive, efficient, and reproducible method, based on solid phase extraction and derivatization with acetic anhydride followed by gas chromatography-mass spectrometry in selected-ion monitoring mode, was developed for the determination of bisphenol A (BPA) in liquid infant formula. The method quantification limit was 0.5 ng g(-1). Extraction recoveries were 85-94% over the concentration range of 2.5-20 ng g(-1). Good reproducibility of the method was observed at levels of 0.54 and 10.4 ng g(-1) with relative standard deviations of 5.0 and 2.8%, respectively. The method was used to analyze samples of 21 canned liquid infant formula products for BPA. BPA was detected in all samples at levels ranging from as low as 2.27 ng g(-1) to as high as 10.2 ng g(-1). The probable daily intakes of BPA due to consumption of canned liquid infant formula were estimated for infants from premature to 12-18 months of age. The maximum probable daily intake of BPA was 1.35 microg kg(-1) of body weight day(-1) for 0-1-month-old infants with the maximum formula intake, which is below the provisional tolerable daily intake for BPA established by Health Canada, 25 microg kg(-1) of body weight day(-1).     

Determination of seven glycidyl esters in edible oils by gel permeation chromatography extraction and liquid chromatography coupled to mass spectrometry detection

A method based on a gel permeation chromatography (GPC) extraction procedure combined with an additional cleanup by solid-phase extraction (SPE) on silica gel and liquid chromatography-mass spectrometry (LC-MS) detection has been validated for the analysis of seven glycidyl esters (GEs) including glycidyl laurate, myristate, palmitate, stearate, oleate, linoleate, and linolenate in various edible oils. This method was conjointly developed and validated by two different laboratories, using two different detection systems, a LC time of flight MS (LC-ToF-MS) and a LC triple-quadrupole MS (LC-MS/MS). The extraction procedure allowed targeting low contamination levels due to a highly efficient matrix removal from the 400 mg oil sample loaded on the GPC column and is suitable for routine analysis as 24 samples can be extracted in an automated and reproducible way every 12 h. GPC extraction combined with SPE cleanup and LC-MS/MS detection leads to a limit of quantification in oil samples between 50 and 100 μg/kg depending on the type of glycidyl ester. Recoveries ranged from 68 to 111% (average = 93%). Quantification was performed by automated standard addition on extracts to compensate matrix effects artifacts. To control recoveries of each sample four isotopically labeled GEs ((13)C(3) or (13)C(4)) were included in the method.     

Determination of bisphenol a and bisphenol B residues in canned peeled tomatoes by reversed-phase liquid chromatography

Bisphenol A (BPA) and bisphenol B (BPB) concentrations were determined in peeled canned tomatoes of different brands bought in Italian supermarkets. Tomato samples analyzed were packaged in cans coated with either epoxyphenolic lacquer or low BADGE enamel. A solid phase extraction (SPE) was performed on C-18 Strata E cartridge followed by a step on Florisil cartridge. Detection and quantitation were performed by a reversed phase high-performance liquid chromatography (RP-HPLC) method with both UV and fluorescence detection (FD). On the total of 42 tested tomato samples, BPA was detected in 22 samples (52.4%), while BPB was detected in 9 samples (21.4%). BPA and BPB were simultaneously present in 8 of the analyzed samples. The levels of BPA found in this study are much lower than the European Union migration limits of 3 mg/kg food and reasonably unable to produce a daily intake exceeding the limit of 0.05 mg/kg body weight, established by European Food Safety Authority.     

锌肥不同施用方式及施用量对我国主要粮食作物增产效果的影响

【目的】施用锌肥是改善作物缺锌、 提高产量和籽粒锌含量的重要措施。锌肥的施用效果受多种因素的影响,通过总结自70年代以来锌肥施用对我国主要粮食作物小麦、 玉米、 水稻产量的影响,分析不同年代、 锌肥施用方式、 锌肥用量对这三大作物产量影响的进程,探讨锌肥的适宜用量和施用方式。【方法】利用万方数据库、 中国知网,查阅了1970至2013年间,我国主要粮食作物水稻、 小麦和玉米锌肥施用相关的田间试验文献333篇,剔除文献中没有产量数据、 没有具体施肥相关信息如施肥量、 施肥方式等文献,有效样本数总计为1656个。采用相关分析、 方差分析等统计分析方法,Microsoft Excel 2010软件分析。【结果】锌肥增产效果受锌肥施用方式、 施用量、 年代的影响,具体结果如下, 1)锌肥施用方式土壤施用、 叶面喷施和种子处理在小麦上的平均增产率分别为11.3%、 10.0%和11.1%; 在玉米上的平均增产率分别为13.7%、 12.7%和12.1%; 水稻上的平均增产率分别为15.0%、 9.8%和9.7%。与叶面喷施和种子处理相比,无论是小麦、 玉米还是水稻,土施锌肥的增产效果最好。2)锌肥施用量小麦、 玉米和水稻的增产率随土施锌肥量增加而增加,当施锌量达到一定量后,随施肥用量的进一步增大,增产率有所降低。小麦、 玉米和水稻土施锌肥的合适用量分别为1545 kg /hm2、 2030 kg/hm2、 2030 kg/hm2。小麦增产率与喷施锌肥的浓度关系不明显,叶面喷施浓度在0.4%~0.5% ZnSO47H2O时增产效果最佳; 而玉米、 水稻增产率和叶面喷施锌肥的浓度变化趋势与土施锌肥变化趋势一致。过去40年玉米和水稻适宜喷施锌肥浓度分别是0.1%~0.3%、 0.2%~0.4% ZnSO47H2O。3)施肥年代随着年代的变化,不同作物施用锌肥的增产幅度不同。随着年代的推进,同一锌肥施用方式在小麦上增产率呈逐渐增高的趋势; 锌肥土施和叶面喷施在玉米上的增产率呈下降趋势; 锌肥土施在水稻上的增产率呈下降趋势,而叶面喷施在水稻的增产率呈先降低后增加的趋势; 种子处理方式在水稻和玉米上的增产率随年代的变化不明显。【结论】施用锌肥能有效提高小麦、 玉米和水稻的产量,但是其增产效果受锌肥施用方式、 施用量、 年代的影响。因此,今后在锌肥施用方面,农户应根据作物、 土壤、 环境等条件,选择恰当的施肥方式及锌肥用量,来提高锌肥的增产效果。     

Determination of multiresidues in rapeseed, rapeseed oil, and rapeseed meal by acetonitrile extraction, low-temperature cleanup, and detection by liquid chromatography with tandem mass spectrometry

A multiresidue method for determining pesticides in rapeseed, rapeseed oil, and rapeseed meal by use of liquid chromatography-tandem mass spectrometry is developed. Samples were extracted with acetonitrile or acidified acetonitrile and cleaned up by a 12 h freezing step. The recovery data were obtained by spiking blank samples at three concentration levels. The recoveries of 27 selected pesticides in rapeseed, rapeseed oil, and rapeseed meal were in the range of 70-118%, at the concentration level of 10 μg kg(-1), with intraday and interday precisions of lower than 22 and 27%, respectively. Linearity was studied between 2 and 500 μg L(-1) with determination coefficients (R(2)) of higher than 0.98 for all compounds in the three matrices. The limits of quantitation (LOQs) of pesticides in rapeseed, rapeseed oil, and rapeseed meal ranged from 0.3 to 18 μg kg(-1). The n-octanol-water partition coefficient showed more influence than water solubility in extracting pesticides by acetonitrile from matrices of high fat content. This method was successfully applied for routine analysis in commercial products.     

长期施肥下我国灌淤土粮食产量和土壤养分的变化

【目的】 灌淤土是我国西北地区重要的粮食和经济作物土壤。了解灌淤土上作物产量的变化,及其对长期施肥的响应,以及灌淤土生产力的变化与其氮磷钾含量的关系,为西北地区作物增产和灌淤土培肥与可持续利用提供理论依据。 【方法】 1988到2004年间,在宁夏银川市、吴忠市、石嘴山市和新疆和田市典型灌淤土区域陆续建立了7个国家耕地质量监测点。2016年,利用时间趋势分析法,探讨了作物产量随时间的变化趋势,分析了长期不施肥和常规施肥条件下,玉米、小麦和水稻产量、产量变异系数、可持续性指数、增产率及地力贡献指数的变化特征,并进一步探讨了增产率与土壤养分的关系。 【结果】 灌淤土上小麦产量随时间呈现递增的趋势,在2004年达到最高 (7.58 t/hm2),之后保持稳定,2016年约为初始年产量的3倍;玉米产量随时间一直呈递增趋势,2016年平均产量为9.8 t/hm2,约为初始年的两倍;水稻产量近年来变化不大。与不施肥相比,常规施肥下小麦、玉米 (28年间) 和水稻 (8年间) 分别平均增产3.43倍、3.20倍和1.21倍,产量可持续性指数分别提高了18.8%、148%和13.9%。监测以来,小麦和玉米农田的地力贡献指数略有下降,但变化不显著。水田的地力贡献指数以每年0.0125的速率增加。28年间,常规施肥使土壤全氮含量从0.4 g/kg提高到1.1 g/kg,有效磷和速效钾含量变化不大。小麦与玉米的增产率与土壤全氮含量呈显著直线正相关关系,小麦、玉米和水稻的平均氮肥农学效率分别为9.8、16.8和27.4 kg/kg。 【结论】 灌淤土上常规施肥 (主要是氮肥)有效提高了玉米、小麦和水稻的产量。土壤全氮含量呈增加趋势,有效磷和有效钾含量基本平稳。土壤肥力对玉米和小麦产量的贡献呈下降趋势,对水稻产量的贡献高且平稳。因此,灌淤土应在合理施用氮肥的同时,注重采取提升地力,实现作物的高产和高效。      

中国主要粮食作物化肥施用量与效率变化分析

2004年至今,在国家支农政策的推动下,农业种植结构大幅度调整,粮食产量连续增加,而且启动了全国测土配方施肥项目。采用2008年的农户调研数据与2001年进行对比,揭示了我国粮食生产体系中化肥效率的变化。结果表明,过去7年中小麦和玉米的单位面积化肥用量分别增加5.4%和29.0%,而水稻减少4.3%。全国粮食作物化肥消费总量增加1.3×106t,但占全国化肥消费总量的比重从68%下降到50%。用PFP(粮食产量除以化肥用量)表征化肥效率,发现三大粮食作物的化肥效率大小排列顺序为水稻小麦玉米;7年中小麦和水稻的化肥偏生产力分别从10.6 kg/kg增加到11.9 kg/kg,13.9 kg/kg增加到15.7 kg/kg,玉米的化肥偏生产力从13.8 kg/kg下降到11.5kg/kg。我国农业种植结构调整对化肥施用量影响较大。粮食作物向优势主产区集中以及机械和管理措施的改善有利于进一步提高粮食作物化肥效率,但经济作物播种面积仍在大幅增加,这将对全国化肥效率变化带来变数。     

Determination of 4(5)-methylimidazole in soy sauce and other foods by LC-MS/MS after solid-phase extraction

A method for the determination of 4(5)-methylimidazole (4MeI) in naturally brewed soy sauce was developed for the first time using solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). SPE on silica-based reversed-phase cartridges with heptafluorobutyric acid as an ion-pairing reagent was used for the efficient cleanup of 4MeI. A multimode ODS column was employed for the chromatographic separation. To subtract the matrix effect during LC-MS/MS analysis, a standard addition method was used. The levels of 4MeI found in naturally brewed soy sauce were extremely low (ranging from <0.002 to 0.023 μg/g), whereas those in soy sauces containing caramel color were generally high (ranging from 0.43 to 4.8 μg/g). The method proved to be useful for the analysis of 4MeI in other foods such as caramel colors, drinks, and Worcestershire sauce.     

Multiwalled carbon nanotubes as sorbent for online solid-phase extraction of resveratrol in red wines prior to fused-core C18-based ultrahigh-performance liquid chromatography-tandem mass spectrometry quantification

An ultrafast analytical protocol based on online solid-phase extraction (SPE)/high-performance liquid chromatography-tandem mass spectrometry for the determination of resveratrol in red wines has been developed. In the present work, multiwalled carbon nanotubes (MWCNTs) were used as SPE sorbents for the analytes' online extraction and cleanup. The target analytes were separated on a fused-core C18-silica column (Halo, 50 mm × 2.1 mm i.d., 2.7 μm) and quantified by triple-quadrupole linear ion trap mass spectrometry in negative ion multiple-reaction monitoring (MRM) mode. The proposed analytical procedures were carefully optimized and validated. The calibration function is linear from 0.37 to 370 ng mL(-1) and from 0.13 to 130 ng mL(-1) for trans- and cis-resveratrol, respectively. The limits of quantification (LOQs) of trans- and cis-resveratrol obtained were 0.05 and 0.06 ng mL(-1), which means that the proposed method is suitable for trace analysis of resveratrol at low-level concentration. At the three fortified levels (low, medium, and high), recoveries of resveratrol ranging from 76.9 to 108.3% were obtained. Eight red wine samples from different regions of China were analyzed. The results indicated that the present online SPE-LC-MS/MS system significantly increased sample throughput and decreased solvent consumption, exhibiting great potential to be applied for analyzing resveratrol in red wines.     

气候变化条件下中国灌溉面积变化的产量效应

灌溉可以有效缓解气候变化对粮食生产的不利影响。采用中国不同区域2006-2019年实际灌溉用水量,对4个气候模式(GFDL-ESM2M,Had GEM2-ES,IPSL-CAM5-LR,MIROC5)驱动下的3种作物模型(GEPIC、PEPIC和LPJml)的灌溉用水量进行评估,优选模拟结果较好的前5个模式组合,分析RCP2.6和RCP6.0情景下,2021-2050年中国玉米、水稻、大豆和小麦产量变化,评估灌溉面积扩张的增产效应。结果显示:未来气候变化下,2021-2050年降水量的增加使得中国水稻和大豆以及北方地区玉米和小麦产量均呈现增长趋势,其中东北80%左右的地区和西北70%左右的地区玉米产量将提高0.2～0.8 t/hm~2,东北85%左右的地区水稻和大豆增产幅度分别超过1.0、0.5 t/hm~2,东北90%左右的地区和西北75%左右的地区小麦产量增幅分别介于1.0～2.0、0.5～1.0 t/hm~2之间。降水量的减少使得西南南部地区的玉米和小麦产量均下降0.2 t/hm~2左右。不同区域玉米和小麦的增产效应差异明显,由于北部地区光热条件较差、小麦基础产量较低,使得小麦灌溉增产潜力(1%～11%)以及增产效率((0.12±0.06)kg/m~3)均较高,北部地区小麦的灌溉面积扩张可有效应对气候变化的不利影响。