螺虫乙酯及其代谢产物在猕猴桃中的残留消解动态

研究建立了螺虫乙酯及其4种主要代谢物在猕猴桃及土壤中的残留分析方法。样品用乙腈提取后,经PSA净化,高效液相色谱质谱联用仪检测,外标法定量。结果表明:在0.01～2.00mg/kg的添加水平下,螺虫乙酯及代谢产物在猕猴桃和土壤中的回收率为73.97%～110.52%,相对标准偏差分别为1.96%～7.91%。采用所建方法,测定螺虫乙酯及代谢产物在猕猴桃和土壤中的残留及消解动态。螺虫乙酯被施用到猕猴桃和土壤中后均迅速降解为B-enol、B-keto。在猕猴桃中螺虫乙酯、B-enol呈逐渐降低的趋势,而B-keto和B-mono呈逐渐升高的趋势;在土壤中螺虫乙酯、B-enol、B-keto均呈逐渐降低趋势,B-mono和B-glu在样品中均没有检出。螺虫乙酯和B-enol在土壤中的降解速度(1.42 d、1.99 d)快于在猕猴桃上的降解速度(4.08 d和6.39 d)。以3000倍液稀释液喷施2次,28 d后,猕猴桃中螺虫乙酯母体的残留量为0.06 mg/kg,高于我国制定的0.02 mg/kg的最大残留限量值,在猕猴桃上的安全使用剂量还需要进一步研究。     

Rapid Residue Determination of Cyenopyrafen in Citrus Peel,Pulp, and Whole Fruit Using Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry

A sample pretreatment method was established to analyze the residues of cyenopyrafen in citrus peel, pulp, and whole fruit using ultra-performance liquid chromatography coupled with tandem mass spectrometry. The target compound was extracted from all matrices with acetonitrile and then cleaned by dispersive solid phase extraction using 10 mg GCB?+?150 mg MgSO₄ for citrus peel; 50 mg PSA?+?150 mg MgSO₄ for citrus pulp, and 50 mg C18?+?50 mg PSA?+?150 mg MgSO₄ for whole fruits. Determination of the target compound was achieved in less than 5.0 min using an electrospray ionization source in positive mode. Average recoveries in citrus peel, pulp, and whole fruit spiked at 0.01, 0.2, and 2 mg kg^?1 ranged from 84.9 to 105.1%, with relative standard deviations (RSD_r) of 0.7–7.9%. The reproducibility (RSD_R) ranged from 2.6 to 6.8%. The limits of detection and quantification ranged from 0.00032 to 0.0012 mg kg^?1 and from 0.0009 to 0.0036 mg kg^?1, respectively. This method was used to determine cyenopyrafen residues in citrus fruits to study its dissipation under field conditions. The trial results showed that the half-lives of cyenopyrafen in whole fruits were 10.2 and 6.2 days in Hunan and Guangxi provinces, respectively. The developed analytical method provides a basis to establish maximum residue limits and monitor cyenopyrafen residue in citrus.     

Fatty acids,tocopherols, phenolic and antioxidant properties of six citrus fruit species: a comparative study

Citrus fruit is a rich source of bioactive phytochemicals. Information on the fatty acid and tocopherol composition of locally grown citrus fruits in Korea is elusive. This work was aimed to study fatty acid, tocopherols, ascorbic acid, antioxidant potential, and selected phenolics from peel and pulp of six citrus species. The most dominant fatty acid was linoleic acid (15–45%), followed by linolenic, palmitic, and oleic acid. Stearic acid was highly abundant in yuzu peel (14.45%) and pulp (15.88%) compared to the other fruits. Unsaturated fatty acids (54–74%) contributed higher composition than saturated fatty acids (25–46%). Peel exhibited better antioxidant potential and contained higher phytochemicals than pulp. The concentrations of α-tocopherol and γ-tocopherol were ranged from 22.96 (yuzu) to 86.93 (cheonhyeyang) and 38.59 (yuzu) ~83.03 (tangerine) μg/g DW, respectively. J-Redhyeyang peel exhibited highest total flavonoids (4.17?±?0.10 mgQE/g DW) and DPPH radical scavenging activity (6.17?±?0.03 mgTE/g DW). FRAP values were highest (20.05?±?0.64 mgTE/g DW) in yuzu peel, while peel of cheonhyeyang was superior in total phenolic contents. Tangerine (3.02?±?0.05 mg/g DW) and yuzu (7.49?±?0.38 mg/g DW) had higher hesperidin concentrations in pulp and peel, respectively. Naringin was found in an appreciable amount in yuzu pulp (2.04?±?0.09 mg/g DW) and peel (6.30?±?0.19 mg/g DW) but not detected in all other fruit species. Our results indicate that citrus fruit peel is the rich source of antioxidant compounds, which can be used to prepare antioxidant rich food product.     

Determination,residue analysis,risk assessment and processing factor of pymetrozine and its metabolites in Chinese kale under field conditions

A simple determination method for pymetrozine and its metabolites in Chinese kale was developed using liquid chromatography with tandem mass spectrometry. The method had good linearity (R² > 0.99), accuracy (recoveries of 73.2–94.1%) and precision (relative standard deviation of 2.5–9.8%). Field results showed that half-lives of pymetrozine were 3.0–4.1 d in Chinese kale, and terminal residue concentrations were all below the United States Environmental Protection Agency’s maximum residue limit (250 μg/kg) at harvest. Owing to risk quotient <100%, pymetrozine is unlikely to give rise to vital health concerns to humans following the recommended application guidelines. Moreover, effects of home processing on pymetrozine residues in Chinese kale were monitored. The processing factor values of four processes were between 0.19 and 0.60, which indicated that the used processes could remove pymetrozine residues from Chinese kale, especially pickling after washing process. The data could provide guidance to safe and reasonable use of pymetrozine and help Chinese governments establish a maximum residue limit for pymetrozine in Chinese kale.     

Dietary exposure of Hong Kong adults to pesticide residues: results of the first Hong Kong total diet study

The use of pesticides and other chemicals has become a common practice in modern agriculture to enhance and stabilise crop yield, protect the nutritional integrity of food, facilitate food storage to assure year-round supplies, and provide attractive and appealing food products. With the adoption of strict good agricultural practice (GAP), only minimal amounts of pesticide residues should remain on the crops or in connected foods of animal origin up the food chain. To assess their associated health risk to local people, the dietary exposure of Hong Kong adults to residues of four groups of pesticides or their metabolites – organophosphorus pesticides (OPPs), carbamates, pyrethrins and pyrethroids, and dithiocarbamate (DTC) metabolites – is estimated in the first Hong Kong Total Diet Study (TDS). A total of 150 commonly consumed food items were collected and prepared “as consumed”. A total of 600 composite food samples were analysed for 85 pesticides or their metabolites by liquid chromatography-tandem mass spectrometry (LC-MS/MS). These pesticides were primarily found at low levels (highest mean = 350 μg kg^?1) in food samples of plant origin such as vegetables and fruits. Dietary exposures to pesticide residues were estimated based on the analytical results and the food consumption data of the local residents. The estimated dietary exposures of Hong Kong adults to all individual pesticides were well below their respective acceptable daily intakes (ADIs). The percentage contributions of the estimated mean and 95th percentile dietary exposures to the ADIs of individual pesticides were <6% and <24% for the OPPs, <1% for the carbamates and pyrethrins and pyrethroids, and <1% and <4% for the DTC metabolites, respectively. The findings indicate that dietary exposures to all the pesticide residues analysed in this study were unlikely to pose unacceptable health risks to the Hong Kong population.     

QuEChERS-超高效液相色谱-串联质谱法测定柑橘中呋虫胺和螺虫乙酯残留量

目的建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定柑橘中咲虫胺及螺虫乙酿残留量的分析方法。方法样品采用QuEChERS方法,经1%甲酸乙腈涡旋振荡提取,无水硫酸镁和氯化钠盐析后,经乙二胺-N-丙基硅烷、C_(18)混合净化剂净化,用Waters ACQUITY UPLC HSS T_3色谱柱分离,超高效液相色谱-串联质谱正离子扫描、多反应监测模式进行测定,外标法定量。结果呋虫胺及其代谢物、螺虫乙酯及其代谢物在相关浓度范围内线性关系良好,相关系数均大于0.99。呋虫胺及其代谢物的回收率为86.8%～97.6%,相对标准偏差为2.7%～6.8%,方法定量限为0.005～0.01 mg/kg;螺虫乙酯及其代谢物的回收率为85.8%～96.9%,相对标准偏差为3.2%～7.4%,方法定量限为0.005～0.008 mg/kg。结论该方法样品前处理过程简单快速,分析时间短,定量限低、正确度及精密度均符合农药残留检测要求,适用于同时测定柑橘中呋虫胺和螺虫乙酯残留。     

食荚豌豆和豌豆中螺虫乙酯及其代谢物残留和膳食摄入风险评估

目的 研究食荚豌豆和豌豆中螺虫乙酯主要代谢物的转化情况,施药措施与残留量的相关性,残留量膳食摄入评估.方法 样品中螺虫乙酯及其代谢物加乙腈提取,N-丙基乙二胺和石墨化碳黑净化,离心,上清液过滤膜后高效液相色谱-三重四极杆串联质谱法检测,对施用过螺虫乙酯的食荚豌豆和豌豆样品进行检测分析及膳食摄入评估.结果 食荚豌豆和豌豆...     

GC-MS法分析杂柑皮中挥发性精油成分

目的:深入了解杂柑皮中挥发性精油成分,探究新品种的研究价值,为柑橘新品种的筛选、加工及皮渣综合利用提供实验依据。方法:采用水蒸气蒸馏法提取3种柑橘品种(玫瑰香柑、JoJo和象山红)中挥发性精油,运用GC-MS法分析挥发性精油成分,用面积归一法确定各组分的相对含量。结果表明:3种品种分别检测出66、68种和61种精油成分,分别占总峰面积的99.37%、99.18%和97.42%。3种品种中共有36种相同的精油成分,其中含量较高的有D-柠檬烯、β-月桂烯、芳樟醇、α-萜品醇、α-蒎烯等。不同的柑橘品种精油成分存在差异,可作为不同品种的重要特征。     

橘皮酱油的制备研究

以大豆、面粉为主要原料,采用高盐稀态发酵技术,并在发酵初期添加柑橘皮渣以生产柑橘酱油。以氨基酸态氮、总黄酮及总多酚含量为主要考察指标确定最优生产条件。研究表明,添加柑橘皮渣20%,酱油中氨基酸态氮含量为1.01 g/100 mL,总黄酮含量为58.87 mg/100 mL,总多酚含量为418.83 mg/100 mL,且增加了21种风味物质。该酱油不仅具有柑橘皮和酱油的营养特性,具有保健功效,还充分利用柑橘生产加工过程中的副产物,提高柑橘皮渣的附加值。     

柑橘皮里功能性物质种类及其提取工艺的研究进展

柑橘类水果是全世界最大宗产量的水果之一,皮渣作为其主要副产物占柑橘总量的20％～40％,具有较大的利用价值。本文综述了柑橘类主要副产品（香精油、果胶、天然色素、膳食纤维、黄酮类化合物和类柠檬苦素）的功能特性,以及国内外对这些物质的提取情况;并对我国柑橘加工产业提出了建议。     

Improvement of Mass Transfer by Freezing Pre-treatment and Ultrasound Application on the Convective Drying of Beetroot (<Emphasis Type="Italic">Beta vulgaris</Emphasis> L.)

The effects of freezing pre-treatment and ultrasound application during drying on microstructure, drying curves, and bioactive compounds of beetroot have been evaluated. Raw and previously frozen (at ? 20 °C) beetroots were convectively dried (40 °C and 1 m/s) with and without ultrasound application using two acoustic densities (16.4 and 26.7 kW/m³), and a diffusional model was proposed to simulate the drying curves. Freezing pre-treatment and ultrasound application caused significant disruptions in the beetroot microstructure and reduced the drying time, enhancing the mass transfer. The external mass transfer coefficient significantly (p < 0.05) increased by 28–49% when ultrasound was applied; moreover, the effective diffusion coefficient significantly (p < 0.05) increased by 60–73% and 204–211%, respectively, due to the ultrasound application on the drying of raw and pre-frozen samples. Freezing caused significant (p < 0.05) increases in betalain and total polyphenol contents and antioxidant activity compared with the raw sample (16–57%), probably due to the release of free forms from the food matrix; meanwhile, drying had the opposite effect (8–54% decrease). Significantly (p < 0.05) higher decreases (32–81%) in bioactive compounds and antioxidant activity were observed when drying was assisted by ultrasound compared with dying without ultrasound. Therefore, freezing pre-treatment and ultrasound application enhanced mass transfer during drying. However, significant changes in quality parameters of the final product were observed.     

三唑磷在柚子茶加工过程中的残留水平变化

为了解柚子茶加工过程中三唑磷残留的变化动态,通过田间喷施5 倍最高推荐剂量的三唑磷溶液以强化农药在柚子上的残留,然后按照柚子茶加工工艺进行加工,采用QuEChERS前处理技术结合气相色谱法检测三唑磷的含量,考察柚子茶加工过程对三唑磷残留量的影响。结果表明：三唑磷主要残留于柚的外果皮中,其残留量为全果的7.3 倍,而果肉中的残留量不足全果的3%。清洗可去除全果中28.5%的残留量;脱苦与浸糖处理均可显著降低外果皮中三唑磷的残留量,其加工因子分别为0.83和0.60;柚子茶成品中三唑磷残留量为0.18 mg/kg,最终加工因子为0.069。     

Evaluation of Microbial Stability,Bioactive Compounds,Physicochemical Properties,and Consumer Acceptance of Pomegranate Juice Processed in a Commercial Scale Pulsed Electric Field System

This paper investigated the feasibility for pasteurizing raw (100 %) pomegranate juice in a commercial scale pulsed electric field (PEF) processing system. The juice was processed at 35 and 38 kV/cm for 281 μs at 55 °C with a flow rate of 100 L/h. Effect of PEF processing on microbial stability, color, °Brix, pH, sediment, antioxidant activity, total phenolic content, anthocyanin, and sensory properties after the treatments and during storage at 4 °C for 12 weeks were studied and compared to those of thermally processed juice. PEF treatments significantly (p?<?0.05) inhibited the growth of total aerobic bacteria, which remained at <2.5 log colony-forming units (CFU)/ml during the 12-week storage. No yeast and mold were detected (<0.69 log CFU/ml) in the PEF-treated juices during storage up to weeks 10 and 12, which is similar to the thermally processed juice. There were no significant differences in pH and °Brix values between the PEF processed juice and unprocessed juice. PEF processing did not alter the contents of total phenolics and anthocyanin as compared to unprocessed juice. PEF processing had significantly (p?<?0.05) less impact on the color of pomegranate juice than thermal processing. PEF-treated juice had the same consumer satisfaction scores as the unprocessed juice, which were significantly (p?<?0.05) higher than thermally processed juice samples. There was no significant difference between the two PEF treatments in all results. This study demonstrated that PEF technology extended microbial shelf-life and preserved the major quality and nutritional characteristics of pomegranate juice, and hence, is technically feasible for commercialization in the juice industry.     

微切变-助剂互作技术制备柑橘皮粉的保健功能研究

目的考察微切变-助剂互作技术制备的柑橘皮粉的保健功能,以促进柑橘皮的合理利用。方法将健康昆明小鼠随机分为空白对照组、粗粉组和微切助粉组,每组10只,空白对照组小鼠饲喂商品鼠粮,实验组小鼠分别饲喂含柑橘皮粗粉或经微切变-助剂互作技术处理柑橘皮制备的微切助粉鼠粮。连续饲养小鼠一定周期后,研究柑橘皮微切助粉对小鼠多种保健功能的影响。结果与对照组相比,柑橘皮微切助粉极显著地增加小鼠的体重,免疫器官指数,血清中抗体Ig G、Ig A和Ig M的含量和血清中SOD的水平,说明柑橘皮可提高小鼠免疫力。二甲苯所致小鼠耳肿胀试验证明柑橘皮微切助粉的耳肿胀抑制率为74.3%,且抗炎效果接近阿司匹林,表明柑橘皮具有非常好的抗炎作用。另外,柑橘皮微切助粉组小鼠的负重游泳时间(6.88±0.27 min)是对照组(4.67±0.18 min)的1.47倍,表明柑橘皮具有抗疲劳作用。与对照组相比,柑橘皮微切助粉极显著地缩短了戊巴比妥钠所致小鼠的入睡时间和延长了睡眠持续时间,表明柑橘皮具有镇静催眠作用。结论柑橘皮具有提高小鼠机体免疫力、抗炎、抗疲劳、镇静催眠的作用,且柑橘皮微切助粉的各种保健效果优于其粗粉。     

利用柑桔皮渣开发膳食纤维的试验

本试验以FMC榨汁后的柑桔皮渣为原料,采用加热加压法提取出柑桔皮渣膳食纤维。对品质分析(以干基％)结果表明:总膳食纤维量达到82.54、SDF:IDF值由0.22提高到0.51,是一种优质膳食纤维源。     

人工接种温州蜜柑后链格孢霉毒素的产生及分布规律

采用超高效液相色谱-串联质谱法结合Qu ECh ERS(quick,easy,cheap,effective,rugged,safe)前处理方法,研究温州蜜柑人工接种链格孢菌(Alternaria alternate)后,病斑部位全果、非病斑部位果皮和果肉中腾毒素(tentoxin,Ten)、链格孢酚(alternariol,AOH)、交链格孢酚单甲醚(alternariol monomethyl ether,AME)、交链孢烯(altenuene,ALT)和细交链格孢菌酮酸(tenuazonic acid,Te A)5种链格孢霉毒素的产生和分布规律。结果表明,病斑部位全果、非病斑部位果皮和果肉中的链格孢霉毒素含量随着病斑直径的扩大,不同链格孢霉毒素的变化趋势不同。Te A、Ten、AME和AOH在所有部位中均有检出,其中Te A检出含量最高,在病斑部位的含量范围为3.05×10~3~55.88×10~3μg/kg,在非病斑部位的含量范围为65.35~40.68×10~3μg/kg;Ten、AME和AOH在病斑部位的含量范围分别为69.16~373.94、22.63~1 395.82μg/kg和8.18~689.19μg/kg;非病斑部位的含量范围分别为0~67.56、0~195.96μg/kg和0~301.91μg/kg;ALT在非病斑部位果肉中未检出,但在非病斑部位的果皮和病斑部位的全果中均有检出,含量最高达16.61μg/kg。研究表明,由于柑橘感染链格孢菌后产生的毒素会从发病部位扩散到健康部位累积,因此,在鲜食加工和风险评估中应引起关注和重视。     

Thermomechanical process intensification for oil extraction from orange peels

The study investigated the intensification and improvement of oil extraction from orange peel through a thermomechanical process: the instantaneous controlled pressure drop (briefly D.I.C. process). This process involves subjecting orange peel for a short time to steam pressure, followed by an instantaneous decompression to a vacuum at 50 mbar. Central composite design was used to study the combined effects of processing steam pressure (1–7 bar; which corresponds to a temperature ranging between 100 °C and 162 °C respectively), processing time (0.3–3.7 min) and initial moisture content of orange peel before thermomechanical oil extraction (9.8–60.2% on dry material basis). The quantitative analysis, have been undertaken on oil present in orange peels, after processing. Correlation analysis of the mathematical regression model indicated that quadratic polynomial model could be employed to optimize the extraction of oil from orange peel. From response surface plots, the three variables exhibited a linear effect with the strongest effect for the processing pressure. The optimum reaction conditions selected with response surface analysis were as follows: steam processing pressure: 6.6 bar, processing time: 3.68 min, initial moisture content: 53.6% d.m. basis. Under these conditions, experimental yield of orange peel oil was close to predicted value (99%) calculated from the polynomial response surface model equation. A kinetic study indicated that extraction performed by D.I.C. process is clearly quicker than conventional steam distillation method.

Industrial relevance

World production of citrus fruit has experienced continuous growth in the last decades of the XX century. Total annual citrus production was estimated at over 105 million tons in the period 2000–2004 (http://www.unctad.org/infocomm/anglais/orange/market.htm). Oranges constitute the bulk of citrus fruit production, accounting for more than half of global citrus production in 2004. Thus, the quantities of generated by-products are very important. In this study, extraction of oil from orange peel was performed through a thermomechanical process developed in our laboratory. We report on some results obtained using this process as well as others comparing extraction kinetics when using a conventional steam distillation process and the proposed extraction process. One of the advantages of the described method is the short contact of extracted oil with the heated zones in the apparatus resulting in a lower heating period of the product compared to steam distillation. At industrial scale, this is interesting regarding oil quality and energy saving.     

阿维菌素和氟啶胺在柑橘汁加工过程中的残留行为及加工因子研究

为评价阿维菌素和氟啶胺在柑橘汁商业化加工过程中的残留行为及加工因子,以普通甜橙为试验材料,以5倍最高推荐施药剂量在重庆和湖南进行田间试验,按照橙汁典型商业化加工过程进行加工,采用QuEChERS前处理结合超高效液相色谱-串联质谱联用技术(UPLC-MS/MS)对各加工单元的农药残留进行检测分析。结果表明,在柑橘汁加工过程中,榨汁是降低阿维菌素和氟啶胺残留最有效的过程;除柑橘皮精油中2种农药发生明显富集外,其余加工产品中农药残留加工因子均小于1。该研究结果可为监测阿维菌素和氟啶胺在柑橘及其制品中的农药残留行为及膳食暴露风险评估提供参考。     

Effect of temperature and some added compounds on the stability of blood orange marmalade

Jams and marmalades are often wrongly believed to be stable products, as the degradation of pigments such as anthocyanins, browning reactions, and the formation of sugar degradation products may occur during storage. The paper aims at studying some of the degradation reactions occurring in blood orange marmalade stored at 20 °C and 35 °C. The addition of natural (tea extract) and naturally occurring (ascorbic acid, cysteine, gallic acid) compounds to marmalade was addressed at investigating the possible effect on retarding such phenomena. Results highlight the dependence of anthocyans and 5-hydroxymethyl-2-furaldehyde (HMF) levels on the storage temperature. Marmalades added with cysteine, unlike the samples added with phenol compounds, showed higher anthocyans and lower HMF levels just after processing, together with a reduced anthocyan loss kinetics and a slowdown of HMF formation during storage at both temperatures. PRACTICAL APPLICATION: Transformation of blood oranges into marmalade represents an alternative to fresh market in periods when the high availability of the citrus causes the collapse of prices. Blood orange marmalade is characterized by a high nutritional value, however, it is not widely distributed yet. Its storability is limited by color and organoleptic changes that influence consumers' acceptance. The optimization of blood orange marmalade preparation could help producers improve storability and widen distribution.     

Lc/Esi/Ms/Ms determination of postharvest fungicide residues in citrus juices

An LC-ESI-MS/MS method was developed for the quantitative detection of postharvest fungicide residues in citrus juices and reported in this paper. The analyses of thiabendazole (TBZ), carbendazim (MBC), thiophanate methyl (TPM), imazalil (IMZ) and prochloraz (PCZ) residues were performed by using a gradient elution in conjunction with positive ionization mode electrospray ionization tandem mass spectrometry. Fungicides were extracted from citrus juices with recoveries ranging from 79.8 to 101.2% and relative standard deviation better than 15%. The quantification limits ranged from 0.01 μg/kg IMZ to 0.06 μg/kg for MBC. The LC-MS-MS method was applied to commercial citrus juices, detecting MBC, TBZ and IMZ residues in the 90% of the samples. Prochloraz residues were detected only in one of the multifruit juice (orange, lemon and carrot) samples.