2015年吉林省市售水果中植物生长调节剂残留量监测结果分析

目的 了解吉林省内市售水果中植物生长调节剂的残留情况,通过对监测数据的分析,为制定食品安全政策法规提供科学依据。方法 2015年从全省九个地区采集75份水果样品,采用 BEH C₁₈(2.1mm×100mm,1.7μm)色谱柱,以乙腈和0.1 % 氨水为流动相,梯度洗脱,流速为0.3mL/min,柱温35°C,多效唑,ESI(+)；赤霉素、2,4-D、噻苯隆、氯吡脲和4-氯苯氧乙酸,ESI(-),在此色谱质谱条件下进行检测。结果 4-氯苯氧乙酸检出率为6.67%,赤霉素检出率10.67%,氯吡脲检出率为18.67%,多效唑检出率为16%,2,4-D检出率为16%,噻苯隆检出率0%,。结论 市售水果中植物生长调节剂残留量检出率比较高,应加大监测力度,通过监测数据的结果分析,采取相应措施以提高食品安全性。     

河北省市售豆芽菜中6种植物生长调节剂 残留调查分析

目的分析调查6种植物生长调节剂在黄豆芽和绿豆芽中残留情况。方法 2014年,应用气相色谱-质谱法对河北省10个区市在本辖区的市场销售的豆芽菜开展了食品安全风险监测,监测项目为4-氯苯氧乙酸、吲哚乙酸、2,4-二氯苯氧乙酸、2,4-二氯苯氧乙酸丁酯、吲哚丁酸、萘乙酸。结果在所检测的52份样品中,其中12份检出4-氯苯氧乙酸、33份检出吲哚乙酸、13份检出吲哚丁酸,其他三项均未检出。检出样品均未超出国家规定的植物生长调节剂的最大残留限量(MRLs)。结论有必要持续监测和控制豆芽中生长调节剂和植物激素的残留,禁防滥用植物生长调节剂给人类健康带来的风险。     

聊城市市售豆芽菜中5种植物生长调节剂残留调查分析

目的 分析聊城市东昌府区市售绿豆芽和黄豆芽中6-苄基腺嘌呤、4-氯苯氧乙酸、2,4-二氯苯氧乙酸、吲哚乙酸、吲哚丁酸的残留情况。方法 样品采用QuEChERs方法提取, 用含有0.1%甲酸的5 mmol/L乙酸铵水(A)和甲醇(B)作为流动相进行梯度洗脱, 质谱采用多反应监测-信息依赖性采集-增强子离子扫描模式(multiple reaction monitoring-information dependent acquisition-enhanced product ion, MRM-IDA-EPI), 同时得到的子离子谱图用于谱图库检索进行定性确证分析。结果 绿豆芽和黄豆芽中均存在植物生长调节剂残留, 在所检测的20份样品中, 10份检出6-苄基腺嘌呤, 11份检出4-氯苯氧乙酸, 20份检出吲哚乙酸, 其他两项均未检出。阳性样品的谱图匹配度均高于70%。结论 市售豆芽中植物生长调节剂的滥用依然存在, 必须持续监测和控制豆芽中植物生长调节剂的残留, 谨防滥用植物生长调节剂给消费者健康带来的风险。     

植物生长调节剂在果蔬中的应用与安全性分析研究进展

植物生长调节剂可有效提高果蔬产量、品质,其在果蔬生产中的应用越来越多;对植物生长调节剂残留危害风险的评估也成为了研究热点。本文综述了植物生长调节剂的主要类别、作用和在果蔬中的应用现状;并归纳分析了果蔬中多效唑、氯吡脲、赤霉酸、乙烯利、2,4-二氯苯氧乙酸（2,4-D）等几种主要生长调节剂的危害和残留现状;发现果蔬中乙烯利的平均残留量最高,葡萄、豆芽、草莓等果蔬中植物生长调节剂残留情况最为严重,其潜在的安全隐患应引起重视;而国家现行植物生长调节剂标准中并未覆盖一些果蔬,亟需完善植物生长调节剂残留相关标准及风险评估。     

农产品中6种植物生长调节剂残留限量标准及 检测方法研究进展

植物生长调节剂是一类具有改善作物品质和调节生长作用的人工合成农药,近年来,调节剂的滥用及使用不当导致的安全问题日益引起关注,因此有必要加强对限量标准的跟踪研究,并进一步提高植物生长调节剂的检测水平。本文综述了农产品生产中常用的氯吡脲、赤霉素、多效唑、乙烯利、矮壮素、2,4-二氯苯氧乙酸这6种常用植物生长调节剂残留检测研究现状,包括农产品中残留限量标准和仪器检测技术等。随着新技术的不断发展和完善,植物生长调节剂残留分析将向多组分、高效率、高特异性、高灵敏度等方向发展。     

云南优势水果中植物生长调节剂残留的膳食摄入与风险评估

目的 明确水果中植物生长调节剂残留的风险, 对水果中植物生长调节剂(plant growth regulator, PGR)残留量实行监测并进行风险评估。方法 整合3年的市场监测数据, 利用农药残留专家联席会议农药急性膳食风险摄入量计算方法和@risk定量风险评估专用软件, 对我国各类人群水果中植物生长调节剂残留膳食摄入风险进行评估。结果 4种水果中均有植物生长调节剂检出, 总检出率为17.50%, 香蕉的检出率最高, 为23.33%, 共有6种PGR成分被检出, 分别为氯吡脲、赤霉素、噻苯隆、2,4-滴、多效唑和乙烯利, 检出率为1.04%~8.96%, 乙烯利最高; 短期膳食摄入结果显示, 4个水果品种消费带来的有检出PGR残留短期膳食摄入量在0.468~32.65 ?g/kg bw/d, 仅占其ARfD的0.38%~65.29%, 均小于100%。结论 植物生长调节剂残留膳食摄入风险虽在不同水果品种、不同风险因子和不同人群之间有差异, 但整体风险水平均在可接受范围内。     

固相萃取-气相色谱法测定水果中氯吡脲

目的 建立固相萃取-气相色谱法(solid-phase extraction and gas chromatography, SPE-GC)检测水果中氯吡脲的方法, 并对猕猴桃、无籽黑提、夏橙和黄心西瓜4种常见水果中氯吡脲的残留进行检测。方法 比较了正己烷、乙酸乙酯、丙酮、甲醇等有机溶剂的萃取效果, 并比较了不同固相萃取小柱的净化效果。结果 萃取溶剂最佳为易分离水层的乙腈, 溶解进样溶剂为丙酮, 溶解度高毒性小且价格经济, 固相萃取小柱选用Florisil柱较好。在此实验条件下, 氯吡脲在0.01~100 mg/L浓度范围内线性良好(r2=0.999893), 检出限为 0.01 mg/kg, 实验回收率在72.8%~90%之间, 相对标准偏差(relative standard deviation, RSD)≤7.9%, 基质效应可以忽略(91.4%~103.0%)。结论 该方法简单准确, 线性范围大, 适用于水果中氯吡脲的残留检测。利用此方法对普洱市某大型超市内猕猴桃等4种水果进行检测, 均未检出氯吡脲, 可见超市水果膨大剂污染很微小。     

水果中常用植物生长调节剂的研究进展

植物生长调节剂是一类具有植物激素活性的人工合成农药,可用于调节水果的生长和贮藏。近年来,由于其在水果生产中的不当或过量使用,而产生的安全事件不断增多。水果中植物生长调节剂的残留问题已经引起社会的广泛关注。本文对水果中5种常用植物生长调节剂(多效唑、赤霉素、氯吡脲、噻苯隆和2,4-D)的理化性质、登记使用、国内外限量以及残留分析方法进行了综述,以期为我国开展水果中植物生长调节剂的限量制定和研究提供参考。     

3种植物生长调节剂在京津冀地区主要瓜果类蔬菜中的残留动态及安全风险评价

目的研究京津冀地区主要瓜果类蔬菜(黄瓜、番茄、甜瓜和茄子等)中的植物生长调节剂残留动态并评价其安全风险。方法调查京津冀地区主要瓜果类蔬菜植物生长调节剂的使用状况,并对京津冀地区12个区县保护地蔬菜产区随机选取的120份样品,进行2,4-D、氯吡脲和4-CPA 3种植物生长调节剂的测定。结果氯吡脲、2,4-D和4-CPA 3种植调剂在黄瓜和番茄样品中均未检出或在检测限以下;在唐山乐亭茄子样品2,4-D残留量检出为7.15μg/kg,唐山乐亭甜瓜氯吡脲残留量为1.01μg/kg,均低于国家标准中的最高残留限量。氯吡脲、2,4-D和4-CPA在黄瓜和番茄模拟残留动态研究结果表明,推荐浓度的氯吡脲在黄瓜上施用7 d后残留量为2.25μg/kg,低于国家最高残留限量标准(0.1mg/kg);推荐浓度的2,4-D和4-CPA在番茄上施用后30 d后残留量分别为225.6μg/kg(低于国家最高残留限量标准0.5 mg/kg)和43.1μg/kg(低于美国限量标准0.05mg/kg)。结论根据调查和模拟试验结果,3种植物生长调节剂在京津冀地区4种蔬菜上不存在安全风险,并提出了降低风险的合理性建议。     

QuEChERS耦合UPLC-MS/MS同时测定葡萄中9种植物生长调节剂

目的:采用液质联用同时测定葡萄中α-萘乙酸、多效唑、2、4-D、矮壮素、吲哚-3-丁酸、6-苄基腺嘌呤、氯吡脲、缩节胺和对氯苯氧乙酸9种植物生长调节剂。方法:样品按Qu ECh ERS方法前处理采用乙腈提取、PSA净化,以乙腈-10 mmol/L乙酸铵(0.05%氨水)溶液为流动相,梯度洗脱,Waters ACQUITY UPLCTMBEH C18(2.1 mm×100 mm,1.7μm)不锈钢色谱柱分离,三重四级杆质谱多反应监测方式检测,外标法定量。结果:9种植物生长调节剂在线性范围内具有良好的线性关系,线性相关性r≥0.99,检出限在0.15~8.89μg/kg,加标回收率在77.2%~112.0%,相对标准偏差在2.08%~9.12%。结论:该方法耗时短、操作简单、有机试剂使用少,灵敏度高、回收率好,适用于日常葡萄中多种植物生长调节剂检测,可缩短检测周期。     

2014~2017年吉林省市售果蔬中植物生长调节剂监测结果分析

目的 调查吉林省内市售果蔬中植物生长调节剂残留情况。方法 2014年~2017年从全省9个地区采集多份果蔬样品, 根据《2014~2017年国家食品污染物和有害因素风险监测工作手册》采用超高效液相色谱-串联质谱法和气相色谱-串联质谱法测定。结果 2014~2017年采集的样品中检出12种植物生长调节剂, 种类检出率达到57.1%。采集的317份样品中, 117份样品检出植物生长调节剂, 检出率达到36.9%。结论 吉林省市售果蔬植物生长调节剂残留存在一定的食品安全问题, 应采取针对措施, 以提高食品安全性。     

Fluctuations in the Levels of Antioxidant Compounds and Antioxidant Capacity of Ten Small Fruits During One Year of Frozen Storage

The fluctuations in antioxidant capacity (2,2-diphenyl-1-picrylhydrazyl, 2,2´-azinobis (3-ethylbenzthiazoline-6-sulphonic acid), and ferric reducing/antioxidant power assays), total phenol, total flavonoid, and total anthocyanin contents of 10 small fruits (sweet cherries, sour cherries, strawberries, red currants, raspberries, blackberries, hawthorn, cornelian cherries, and red and white grapes) were monitored during storage at ?20°C. After one year in storage, all varieties except hawthorn and white grapes retained equal or slightly greater total phenol content in comparison to the initial values. The total flavonoid and total anthocyanin levels also remained stable or even increased after 12 months in all fruits exept hawthorn and strawberries. Red currants and raspberries exhibited optimal preservation of antioxidant capacity, while hawthorn showed a decrease in the antioxidant capacity during different time points in storage as well as at the end of storage. Analyzed fruits were classified into four main groups based on hierarchical cluster analysis.     

Simultaneous Determination of Seven Plant Growth Regulators in Melons and Fruits by Modified QuEChERS Coupled with Capillary Electrophoresis

A capillary electrophoresis method for the simultaneous determination of seven plant growth regulators including gibberellic acid, abscisic acid, 3-indole acetic acid, 3-indolepropionic acid, 3-indolebutyric acid, 2,4-dichlorophenoxyacetic acid, and 2-methyl-4-chlorophenoxyacetic acid in melons and fruits was established and validated. The samples were ultrasonically extracted with acidified acetonitrile and then dehydrated. The resulting solution was purified with modified QuEChERS method, and then dried-up under weak nitrogen flow, and the residue was redissolved with methanol-water (1:4, v/v) as sample solution. The electrophoretic separation was performed in an uncoated fused-silica capillary with borax buffer (pH 10.5) containing 29% of ethanol as the running buffer. The running voltage was 25 kV with the column temperature of 30 °C. The linear ranges of gibberellic acid, abscisic acid, and 2-methyl-4-chlorophenoxyacetic acid were from 0.10 to 8.0 μg/mL, while the others were from 0.05 to 4.0 μg/mL with the correlation coefficients greater than 0.997. The limits of detection and the limits of quantification of the method were in the range of 1.54–5.76 and 5.12–19.2 μg/kg, respectively. The recoveries of the method ranged from 69.0 to 109% with the relative standard deviations ranging from 2.01 to 15.4%. The proposed method has been successfully applied to the determination of plant growth regulator residues in 15 melon and fruit samples, and gibberellic acid and abscisic acid were detected in the samples.     

Mold growth on strawberries and cherries during storage at 25 degrees C

Mold species that grew on the surface of retailed strawberries (10 packs, 211 strawberries) and cherries (18 packs, 441 cherries) during storage at 25 degrees C were isolated and identified to evaluate the state of mold growth. Mold growth was observed on 208 (98.6%) of the 211 strawberries and 193 (43.8%) of the 441 cherries. The mold species most frequently isolated from strawberries was Botrytis cinerea, being observed in 81.0% of the strawberries examined, followed by Cladosporium and Alternaria alternata. The mold most frequently isolated from cherries was Alternaria (28.7%), followed by Penicillium, Botrytis, and Cladosporium. The frequency of cherries on which mold growth was observed varied among packs. Mold tended to grow more often in the areas of the fruits in contact with adjacent fruits.     

Residues of insecticides, and fungicides in fruit produced in Ontario, Canada, 1986-1988

Between 1986 and 1988, 306 composite samples of fruit representing eight commodities were collected from farm deliveries to the marketplace in Ontario, Canada. All samples were analysed for insecticides and fungicides. The analysis procedure included tests for organochlorine, organophosphorus, synthetic pyrethroid and methylcarbamate insecticides and dithiocarbamate, dicarboximide and organochlorine fungicides. The commodities tested included apples, blueberries, cherries, grapes, peaches, pears, raspberries and strawberries. In 14% of all fruit samples, pesticide residues were below the detection limits, which ranged between 0.005 and 0.02 mg/kg. A further 14% had total combined pesticide residues below 0.1 mg/kg. Total combined fungicide and insecticide residues ranged from 0.1 to 11 mg/kg in 72% of samples. Six different pesticides were in violation of maximum residue limits (MRL) on 11 (3.6%) of fruit samples. Captan exceeded the 5 mg/kg MRL in five samples and EBDC exceeded the 7 mg/kg MRL in two. Other violations included single fruit samples with dicofol, endosulphan, phosalone and iprodione above the MRL. Raw grapes harvested for wine contained residues of 10 pesticides and the number changed little following the crushing of the grapes; however, fermentation into wine significantly reduced residues. Six insecticides and four fungicides were present on the raw grapes and 4/105 were above the MRL. Following crushing, four insecticides and five fungicides were identified and 4/40 were above the MRL. In wine only three insecticides were identified and all were well below the MRL. Carbaryl appeared to be the most persistent, declining very little between raw grapes and wine.     

植物生长调节剂对番茄产量和品质的影响及膳食摄入风险评估

目的 明确不同植物生长调节剂赤霉酸、2,4-滴和噻苯隆对番茄产量和品质的影响, 掌握它们在番茄中的残留情况以及对不同人群的膳食摄入风险。方法 在番茄花期施用植物生长调节剂赤霉酸、2,4滴和噻苯隆各1次, 正常成熟期采摘, 分析不同植物生长调节剂处理对番茄产量和品质的影响及残留情况, 整合两年的番茄市场监测数据, 利用农药残留专家联席会议农药急性膳食风险摄入量计算法和@risk定量风险评估软件, 对番茄中3种植物生长调节剂残留在我国不同人群中的膳食摄入风险进行评估。结果 3种植物生长调节剂均可显著提高番茄的产量和品质(P<0.05), 其中噻苯隆效果最显著, 且产品中相应植物生长调节剂残留量较低, 平均值0.0042~0.0058 mg/kg; 3种植物生长调节剂在市场监测的300个样品中均有检出, 总检出率9.33%, 检出平均值0.034~0.069 mg/kg; 番茄中赤霉酸、2,4-滴和噻苯隆残留的短期膳食摄入量在0.00104~ 0.00658 mg/kg bw/d, 仅占相应每日急性参考剂量的0.60%~7.24%, 急性风险较低。结论 在番茄花期施用赤霉酸、2,4-滴或噻苯隆可显著提高番茄的产量和品质, 且产品中残留量低, 番茄中3种植调剂残留在不同人群中的膳食摄入风险均很低, 在可接受范围内。