吡唑醚菌酯与苯醚甲环唑混剂对花生褐斑病的防治

[目的]明确吡唑醚菌酯和苯醚甲环唑混合对花生褐斑病毒力增效作用。[方法]室内联合毒力测定和田间药效试验。[结果]筛选得到吡唑醚菌酯与苯醚甲环唑的增效型混剂。[结论]吡唑醚菌酯与苯醚甲环唑以1:1混配对抑制菌丝生长增效最为明显,共毒系数为138.86。田间药效试验中,20%吡唑醚菌酯·苯醚甲环唑悬浮剂对花生叶斑病的防治效果达到84.50%,显著优于2个单剂的防效。     

吡唑醚菌酯在杨桃中残留检测及膳食风险评估

目的建立了吡唑醚菌酯在杨桃中的残留检测方法,并对杨桃中的残留量进行膳食摄入评估,为我国吡唑醚菌酯在杨桃中的残留限量设定提供参考。方法 样品经乙腈提取,C18和PSA净化,液相色谱串联质谱法检测,外标法定量。结果 在不同添加水平下,杨桃中吡唑醚菌酯的平均回收率为73%～105%,相对标准偏差(RSD)为4.2%～7.5%,最小检出量为1×10_^-9 mg,最低检测浓度为0.01 mg/kg。吡唑醚菌酯在杨桃中的消解符合一级动力学方程,半衰期为5.7～5.8 d。按本试验设计进行施药,不同采收间隔期杨桃中吡唑醚菌酯的残留量均<2.56 mg/kg。结论 我国并未制定吡唑醚菌酯在杨桃上的最大残留量,参照杨桃相似的热带水果杨梅中吡唑醚菌酯的残留量设定：吡唑醚菌酯的普通人群国家估计每日摄入量(NEDI)是1.2 mg,占日允许摄入量的63.3%左右,认为对一般人群健康不会产生不可接受的风险。     

蔬菜中多效唑残留的膳食暴露与风险评估

多效唑是蔬菜种植中常用的延缓类生长调节剂。为明确蔬菜中多效唑残留的膳食摄入风险,开展了马铃薯、番茄和茄子3个蔬菜品种的规范残留试验和市场抽样监测,并基于以上数据对蔬菜中多效唑残留进行了膳食摄入慢性风险和急性风险评估,提出了蔬菜中多效唑的推荐MRL值。结果表明,蔬菜中多效唑的国家估计每日摄入量为0.040~0.21μg/(kg bw·d),仅占ADI的0.04%~0.21%,国家估计短期摄入量为0.070~0.95μg/(kg bw·d),仅占ARf D的0.07%~0.95%,基于规范残留试验和市场监测得到的评估结果相一致,蔬菜中多效唑残留对我国各类人群的膳食摄入慢性风险极低,急性风险水平虽在不同人群和不同蔬菜品种中有差异,但整体风险也非常低,均在可接受范围内;蔬菜中多效唑残留的建议MRL值为0.5 mg/kg,该值对我国各类人群多效唑暴露的保护水平为12.5~50倍。     

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。     

吡唑醚菌酯在枇杷中的残留行为及膳食风险评估

目的 探明吡唑醚菌酯在枇杷中的残留特性,评价其使用安全性。方法 样品经乙腈提取, N-丙基乙二胺分散吸附剂净化, 0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱, 超高效液相色谱-串联质谱多反应监测模式检测,采用基质匹配标准溶液外标法定量。采用超高效液相色谱-串联质谱检测枇杷中的吡唑醚菌酯的残留量,进行膳食风险评估。 结果 在0.01、0.10、1.00和3.00 mg/kg添加水平下,吡唑醚菌酯在枇杷样品中的平均添加回收率在92%~96%之间,相对标准偏差范围为3.3%~5.4%,定量限为0.01 mg/kg。吡唑醚菌酯在枇杷中的消解半衰期为9.5~12.8 d。风险评估结果表明,我国普通人群摄入吡唑醚菌酯的风险概率为60.3%。不同年龄段人群膳食摄入评估结果表明显示,随采收间隔期的延长及年龄增加,风险概率逐渐降低。结论 30%吡唑醚菌酯悬浮剂,按推荐剂量(有效成分 250 mg/kg)施药2次,施药间隔7 d,推荐安全间隔期为14 d。在此条件下,其对我国一般人群产生的风险在可接受范围内。     

吡唑醚菌酯在小麦上的残留分析及安全性评价研究

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography/tandem mass spectrometry,UPLC-MS/MS)测定小麦中吡唑醚菌酯的含量,研究其在小麦籽粒和秸秆中的残留状况及消解规律,评估吡唑醚菌酯的膳食风险。方法实验样品经乙腈提取、净化后,经Waters Acquity UPLC BEH C_(18)柱(50 mm×2.1 mm,1.7μm)分离,以0.1%甲酸水-甲醇为流动相进行梯度洗脱;流速为0.3 mL/min,多反应监测模式监测。结果吡唑醚菌酯在0.0005-0.20 mg/mL的范围内线性关系良好,相关系数大于0.999,小麦籽粒、小麦秸秆不同添加水平下的平均回收率范围为66%～97%、88%～98%,相对标准偏差分别为1.9%～5.5%、1.2%～12.4%,定量限为0.01 mg/kg。吡唑醚菌酯在小麦籽粒中的残留消解符合一级动力学方程,其消解半衰期为2.74～5.82 d;用药后小麦籽粒中吡唑醚菌酯的最终残留未检出～0.10 mg/kg;膳食风险评估表明,末次施药21 d后吡唑醚菌酯的国家估算每日摄入量是1.0874 mg,风险概率为57.53%。结论吡唑醚菌酯在小麦中的消解速度较快,虽不能在小麦中完全降解,但通过膳食评估发现长期膳食摄入对人体健康不会产生不可接受的风险。     

QuEchERS/GC-MS快速检测番茄中苯醚甲环唑残留

建立了番茄中苯醚甲环唑残留的快速检测方法。样品采用改进的Qu Ech ERS方法进行提取和净化,提取液使用GC-MS检测。结果表明,苯醚甲环唑在0.01μg/m L~0.20μg/m L范围内具有良好的线性关系,相关系数为0.999,样品中苯醚甲环唑添加水平为0.05 mg/kg、0.10 mg/kg、0.5 mg/kg时,平均回收率为87.6%、90.4%、98.0%,相对标准偏差在3.8%~8.1%之间。本方法操作简便、快速、高效,适用于番茄中苯醚甲环唑的快速筛查与检测。     

UPLC-MS/MS法测定糙米和稻壳中吡唑醚菌酯残留

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)法测定糙米和稻壳中吡唑醚菌酯残留的方法。样品中吡唑醚菌酯经乙腈水溶液提取、弗罗里硅土柱净化后,以C_(18)反相柱为分析柱,甲酸水溶液-甲醇为流动相,在多反应监测模式下进行质谱检测,采用电喷雾正离子源,外标法定量。吡唑醚菌酯在0.02~0.50 mg/L范围内与峰面积呈良好线性关系,线性方程为:y=77425 x+630.82,相关系数的平方为0.9979。向空白糙米、空白稻壳中分别添加吡唑醚菌酯标样,使其添加量分别为0.02、0.05、0.10 mg/kg时,平均回收率分别为84.7%~101.0%和86.2%~102.5%,相对标准偏差分别为3.7%~4.9%和5.8%~8.1%。糙米和稻壳中吡唑醚菌酯的最低检测限均为0.2μg/kg。该方法的灵敏度和准确度都较高,适合于糙米和稻壳中吡唑醚菌酯的残留分析。     

云南省三七花、三七须根中9种杀菌剂含量监测结果分析

目的 了解云南地区三七花、三七须根中丙环唑、噁霜灵、腈菌唑、醚菌酯、腐霉利、多菌灵、嘧霉胺、苯醚甲环唑、甲霜灵9种杀菌剂污染状况。方法 按照《云南省食品安全风险监测方案》中样品采集要求, 在云南8个地区采集62个样品。按照《国家食品污染物和有害因素风险监测工作手册》对多菌灵、嘧霉胺、苯醚甲环唑、甲霜灵进行检测及国家标准GB 23200.113-2018《食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定》对丙环唑、噁霜灵、腈菌唑、醚菌酯、腐霉利进行检测。结果 9种杀菌剂中, 苯醚甲环唑、嘧霉胺、甲霜灵、多菌灵超标率较高, 分别为16.1%, 14.0%, 12.9%, 4.84%。丙环唑、噁霜灵、腐霉利超标率为3.23%, 腈菌唑、醚菌酯未超标。结论 云南地区三七花、三七须根中杀菌剂污染超标率较高, 应采取措施加以控制。     

桃胶中多农药残留分析及风险评估

目的:研究桃胶中农药残留及风险。方法:基于液相色谱—串联质谱法(LC-MS/MS)建立桃胶中44种农药残留的定量分析方法,并对全国173份桃胶样品进行农药残留检测和风险评估分析。结果:基于LC-MS/MS农药残留检测方法的检出限(LOD)为0.05～1.80μg/kg,定量下限(LOQ)为0.20～2.42μg/kg,加标回收率为61.77%～119.48%。桃胶样品中共检出22种农药,农药总检出率为98.8%,平均每个样品检出农药次数为2.8次,苯醚甲环唑检出率最高(95%),其次是毒死蜱(54%)、多菌灵(34%)、呋虫胺(32%)、吡唑醚菌酯(19%)等。不同桃胶样品中苯醚甲环唑平均残留量最高为0.332 mg/kg,其次是呋虫胺(0.093 mg/kg)、多菌灵(0.061 mg/kg)、毒死蜱(0.033 mg/kg)。结论:桃胶中农药的残留与桃生产用药有关,其残留量总体处于低风险水平,推荐8—10月份采摘桃胶。     

2012~2019年云南省蔬菜中毒死蜱膳食摄入风险评估

摘 要: 目的 了解云南省蔬菜中毒死蜱残留水平, 评估蔬菜中毒死蜱膳食暴露风险。方法 2012~2019年采集云南省市售蔬菜进行毒死蜱测定, 结合我国食物消费量数据, 采用点评估方法对毒死蜱进行急、慢性膳食暴露评估, 评估结果与急性参考剂量(acute reference dose, ARfD)、每日允许摄入量(acceptable daily intake, ADI)进行比较, 从而评价蔬菜中毒死蜱的暴露风险。结果 1~4岁人群的急性暴露量大于ARfD(0.1 mg/kg bw), 其余年龄组的急性暴露量均小于ARfD(0.1 mg/kg bw); 各年龄组平均暴露量低于ADI(0.01 mg/kg bw)。结论 蔬菜中毒死蜱的慢性暴露风险低, 但需关注急性暴露风险。     

Organophosphorus pesticide residues in Greek virgin olive oil: levels, dietary intake and risk assessment

The occurrence of organophosphorus pesticide (OPs) and their metabolite residues was investigated in 167 samples of Greek virgin olive oil during a 2-year (2004-2005) sampling campaign. A total of 30.5% of samples contained detectable residues, although only one sample contained dimethoate residues above the maximum residue limit. Among the seven detected OPs, fenthion and fenthion sulfoxide residues were detected in 10.8 and 14.4% of the samples, respectively, at levels of 0.003-0.61 mg kg(-1). Dimethoate was detected in 10.2% of the samples at 0.003-0.057 mg kg(-1). The acute dietary risk assessment was undertaken by determining the national estimated short-term intake (NESTI); for chronic dietary risk assessment, the national theoretical maximum daily intake (NTMDI) and national estimated daily intake (NEDI) were calculated. The estimated intakes (NESTI and NEDI) of each pesticide were <7 and <0.86% of the corresponding acute reference doses (ARfDs) and acceptable daily intakes (ADIs), respectively. A cumulative risk assessment was performed using the hazard index (HI) and toxicity equivalence factor (TEF), taking into account that OPs share the same toxicological mechanism. The determined HI and TEF values were found to represent only a small portion of the respective ADIs or ARfDs. These results indicate that there is neither acute nor chronic risk for the Greek population through olive oil consumption.     

Intake of saccharin, aspartame, acesulfame K and cyclamate in Italian teenagers: present levels and projections

The intake of saccharin, aspartame, acesulfame K and cyclamate was assessed in 212 Italian teenagers aged 13-19 in 1996. Total daily intake of intense sweeteners was assessed on the basis of dietary records (14 consecutive days). The sweetener content of sugar-free products (soft drinks, candies, chewing gums, yoghurts, jam and table-top sweeteners) was provided by manufacturers. Sugar-free products were consumed by 77% of the subjects. Mean daily intake among consumers was 0.24mg/kg body weight (bw) for cyclamate (13 subjects), 0.21mg/kg bw for saccharin (9 subjects), 0.03mg/kg bw for aspartame (162 subjects), and 0.02mg/kg bw for acesulfame K (56 subjects). No subject exceeded the ADI (Acceptable Daily Intake) of an intense sweetener. Projections based on the present levels of use of intense sweeteners in sugar-free products and on the dietary pattern observed in the sample suggest that approaching the ADI could be possible only if subjects with high intakes of both soft drinks and table-top sugar substituted these items with respectively sugar-free beverages and table-top sweeteners containing either saccharin or cyclamate.     

蔬菜中植物生长调节剂残留的膳食暴露与 风险评估

目的为明确蔬菜中植物生长调节剂(plant growth regulator,PGR)残留的风险,对蔬菜中植物生长调节剂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(JMPR)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,对我国各类人群蔬菜中植物生长调节剂残留膳食摄入风险进行评估。结果蔬菜中植物生长调节剂的残留量较低,为0.0109~0.182 mg/kg,辣椒中主要检出矮壮素和甲哌啶残留,番茄中主要检出2,4-滴残留,马铃薯中主要检出甲哌啶和矮壮素残留;短期膳食摄入结果显示,辣椒、番茄和马铃薯3个蔬菜品种消费带来的有检出PGR残留短期膳食摄入量在0.0957~11.0?g/(kg bw·d),仅占其急性参考剂量的0.0319%~22.0%,急性风险较低。结论蔬菜中植物生长调节剂残留膳食摄入风险虽在不同蔬菜品种、不同风险因子和不同人群之间有差异,但整体风险水平不高,均在可接受范围内。     

Exposure of consumers to deoxynivalenol from consumption of white bread in Hungary

In view of the frequent occurrence of mycotoxins in cereals, a study was initiated to assess the exposure of the Hungarian adult population. Consumption data for 1360 individuals, based on a 3-day questionnaire, indicated that white bread accounted for the major intake of cereal-based products. Various cereal products were analysed for 16 mycotoxins by a LC/MS/MS multi-toxin method with LOD of 16 μg kg?1 and LOQ of 50 μg kg?1. Deoxynivalenol (DON) was most frequently detected, but no acetyl-deoxynivalenol was present in detectable concentrations. Consumer exposure was calculated with standard Monte Carlo probabilistic modelling and point estimates, taking into account bread consumption and DON contamination in independently taken wheat flour and wheat grain samples. Over 55% of cases the DON intake were below 15% of the provisional maximum tolerable daily intake (PMTDI) of 1 μg/(kg bw)/day. However, in 5-15% of cases, the intake from bread consumption alone exceeded the PMTDI. Wheat grain data led to the higher percentage. Intakes estimated from both data sets were at or below the acute reference dose (ARfD) of 8 μg/(kg bw)/day in 99.94-99.97% of cases.     

Organophosphorus pesticide residues in Greek virgin olive oil: levels,dietary intake and risk assessment

The occurrence of organophosphorus pesticide (OPs) and their metabolite residues was investigated in 167 samples of Greek virgin olive oil during a 2-year (2004–2005) sampling campaign. A total of 30.5% of samples contained detectable residues, although only one sample contained dimethoate residues above the maximum residue limit. Among the seven detected OPs, fenthion and fenthion sulfoxide residues were detected in 10.8 and 14.4% of the samples, respectively, at levels of 0.003–0.61 mg kg^?1. Dimethoate was detected in 10.2% of the samples at 0.003–0.057 mg kg^?1. The acute dietary risk assessment was undertaken by determining the national estimated short-term intake (NESTI); for chronic dietary risk assessment, the national theoretical maximum daily intake (NTMDI) and national estimated daily intake (NEDI) were calculated. The estimated intakes (NESTI and NEDI) of each pesticide were <7 and <0.86% of the corresponding acute reference doses (ARfDs) and acceptable daily intakes (ADIs), respectively. A cumulative risk assessment was performed using the hazard index (HI) and toxicity equivalence factor (TEF), taking into account that OPs share the same toxicological mechanism. The determined HI and TEF values were found to represent only a small portion of the respective ADIs or ARfDs. These results indicate that there is neither acute nor chronic risk for the Greek population through olive oil consumption.     

广东省居民面制食品中铝的暴露评估研究

目的：了解广东省面制食品中铝污染的状况,并对居民来源于面制食品的铝摄入状况进行暴露评估。方法：2009年从广东省21个地市的超市、食杂店、集贸市场等随机采集面包、馒头、包子以及油饼油条类食品共840份,按照国家标准GB/T5009.182—2003《面制食品中铝的测定》方法测定其中的铝含量。将2002年广东省居民膳食营养与健康状况监测的调查人群按照不同的年龄、性别分成10组,分别计算面制食品消费量平均值和第97.5百分位数（P97.5）情况下各组人群铝的摄入情况。结果：面制食品中铝平均含量为210.30mg/kg,调查人群来自面制食品的平均铝摄入量0.10mg/（d.bw）,为每日可耐受摄入量（Acceptable Daily Intake,ADI）的0.73倍,从总体上看,2002年广东省营养与健康状况监测调查人群来源于面制食品的铝摄入水平是安全的。面制食品消费量为第97.5百分位数的情况下,调查人群总的铝摄入量为0.61mg/（d.bw）,为ADI的4.35倍,各组的铝摄入量平均值和第97.5百分位数铝摄入量分别为ADI的0.61—2.49倍、3.05—14.78倍,超出ADI倍数最高者为组1的2—7岁少年儿童。结论：需要关注广东省居民膳食铝食用安全情况,尤其是对生长发育阶段的少年儿童。在此基础上,尚需要纳入其它含铝高的食物调研,进行更加精细和全面的膳食铝健康危害风险评估。     

葱、姜、萝卜和豇豆中戊唑醇残留检测及膳食风险评估

[目的]研究葱、姜、萝卜、萝卜叶和豇豆中戊唑醇残留检测方法,分析4种蔬菜中残留量差异,并对最终残留量进行长期膳食摄入和急性膳食摄入风险评估。[方法]样品中戊唑醇采用QuEChERS前处理方法进行提取,高效液相色谱-三重四极杆串联质谱法检测;采用IBM SPSS Statistics 23分析4种蔬菜中残留量差异,运用膳食摄入风险评估模型进行急性膳食摄入和长期膳食摄入风险评估。[结果]当添加水平是0.01、0.1和1 mg/kg时,葱、姜、萝卜、萝卜叶和豇豆的平均回收率分别为100%～117%、101%～112%、94%～99%、102%～111%和92%～95%,相对标准偏差分别为2.0%～3.8%、1.8%～7.6%、2.3%～4.3%、1.4%～7.7%和5.7%～6.9%。葱、姜、萝卜、萝卜叶和豇豆中戊唑醇残留量分别为<0.01～0.014 mg/kg、<0.01～0.042 mg/kg、<0.01～0.023 mg/kg、0.057～4.13 mg/kg和<0.01～0.079 mg/kg。第1次采收和第2次采收时,萝卜叶与其它4种基质中残留量均存在差异,但差异不显著。戊唑醇的普通人群国家估计每日摄入量是0.455 mg,占日允许摄入量的24.1%左右。葱、姜、萝卜、萝卜叶和豇豆中戊唑醇的国家估计短期摄入量分别为0.0337、0.000432、0.000562、0.0169、0.000532 mg/kg bw,占急性参考剂量百分比分别为0.112%、1.44%、1.87%、56.3%和1.77%。[结论]按该试验的施药方式进行施药时,最终残留量差异与作物种类相关,试验蔬菜中戊唑醇的残留量对一般人群健康风险在可接受的范围内。     

饼干中苯甲酸及其钠盐含量分析及其膳食暴露评估

对市场中210个饼干样品进行苯甲酸及其钠盐含量用HPLC方法进行测定,并对检测数据采用膳食暴露评估方法,评估城市居民的膳食风险。结果显示,婴儿(6～12个月)膳食暴露量为12.25～31.62μg/kg bw·d,其97.5/99百分位值的膳食暴露量为73.99～195.62μg/kg bw·d,建议婴儿(6～12个月)少量食用或食用不含苯甲酸的婴儿饼干。对于1～3岁的幼儿其膳食暴露量为10.25～13.25μg/kg bw·d,在97.5/99百分位值的膳食暴露量为105.24～139.10μg/kg bw·d,食用此类食品的风险是可以接受的。对于3岁以上人群食用此类食品的风险比1～3岁幼儿更小,风险程度更低。另外,饼干中威化和酥性类饼干中苯甲酸的残留水平相对于其他类饼干含量略高,而发酵和韧性类的饼干中苯甲酸的含量相稍低;同时显示江苏产的产品质量相对较好。