丁硫克百威在豇豆不同时期施用的降解代谢研究

为明确丁硫克百威在豇豆播种期、苗期、结荚期使用后的降解代谢,以及可能产生的膳食风险,分别以其在蔬菜上登记的最低剂量、最高剂量、最高剂量的1.5倍3种剂量施药,进行田间模拟残留试验。将采集的成熟豇豆通过乙腈提取、C18分散净化,经超高效液相色谱串联质谱方法检测,测定豇豆中丁硫克百威及其代谢物——克百威和3-羟基克百威的残留量。结果表明,丁硫克百威、克百威和3-羟基克百威在豇豆中的定量限均为0.01 mg·kg^-1,在0.01~1 mg·kg^-1的添加水平下,丁硫克百威、克百威和3-羟基克百威的平均回收率为72%~105%,相对标准偏差为1.4%~20.1%。丁硫克百威使用后的超标风险主要源于其代谢物——克百威和3-羟基克百威。播种期施药后的豇豆样品均无丁硫克百威及其代谢物检出;苗期以最高剂量的1.5倍施药后,第10天的样品中克百威(含3-羟基克百威)的残留值超出中国国家标准中规定的最大允许残留限量(MRL);结荚期2次或3次施药后7 d内克百威(含3-羟基克百威)的残留值超出MRL。结荚期施药时,丁硫克百威在2次施药和3次施药后的慢性膳食摄入风险和急性膳食摄入风险均较低,小于100%;但克百威(含3-羟基克百威)的急性膳食摄入风险较高,以最高剂量的1.5倍2次施药或3次施药后,克百威(含3-羟基克百威)的急性膳食摄入风险于药后7 d才降至100%以下。综上,播种期使用丁硫克百威不会导致豇豆中残留超标,可以安全使用;但苗期和结荚期使用丁硫克百威存在极高的风险,应禁止其在播种期以外的使用。     

Proportionality principle revisited – relationship between application rates and pesticide residue concentrations in food commodities

BACKGROUND

The proportionality principle has been broadly used for over 10 years in regulatory assessments of pesticide residues. It allows extrapolation of supervised field trial data conducted at lower or higher application rates compared to the use pattern under evaluation by adjustment of measured concentrations, assuming direct proportionality between the rates applied and the resulting residues. This work revisits the principle idea by using supervised residue trials sets conducted under identical conditions but with deviating application rates. Four different statistical methods were used to investigate the relationship between application rates and residue concentrations and to draw conclusions on the statistical significance of the direct proportionality assumed.

RESULTS

Based on over 5000 individual trial results, the assumption of direct proportionality was not confirmed to be statistically significant (P > 0.05) using three models: direct comparison of application rates and residue concentrations ratios and two linear log-log regression models correlating application rate and residue concentration or only residue concentrations per se. In addition, a fourth model analysed deviations between expected concentrations following direct proportional adjustment and measured residue values from corresponding field trials. In 56% of all cases, the deviation was larger than ±25%, which represents the tolerance usually accepted for the selection of supervised field trials in regulatory assessments.

CONCLUSION

Overall, the assumption of direct proportionality between application rates and resulting residue concentrations of pesticides was not statistically significant. Although the proportionality approach is highly pragmatic in regulatory practice, its use should be considered carefully on a case-by-case basis. © 2023 The Authors. Pest Management Science published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.     

欧盟、美国和日本加工农产品中农药残留评估现状

本文介绍了欧盟、美国和日本评估加工农产品中农药残留的数据要求和试验准则,以及开展膳食摄入风险评估和推荐农药最大残留限量(MRL)的方法,汇总了用于农药残留评估的加工农产品及其分类,分析了加工农产品中农药MRL制定现状,为进一步提高我国相关领域技术提供借鉴。比较分析结果表明,欧盟和美国在农药登记资料要求中明确提出了加工试验数据要求并且制定了相应的试验准则,美国在试验准则中描述了加工农产品中农药MRL的推荐原则;美国和日本制定了一定数量的加工农产品中农药MRL,欧盟建立了适用于监管农药MRL的加工因子数据库;欧盟、美国和日本均在相关法规中规定了加工农产品中农药残留的合规性判定。     

吡蚜酮在马铃薯中的残留与膳食风险评估

为评价马铃薯中吡蚜酮残留引发的膳食风险。2016年-2018年开展了3年12地规范残留试验,构建吡蚜酮在马铃薯中的残留检测方法,并对我国一般人群进行了膳食风险评估。马铃薯样品使用2%乙酸乙腈提取,C18净化,外标法定量,UPLC-MS/MS检测。在0.01～1 mg/kg添加水平下,吡蚜酮在马铃薯中的平均回收率为75%～85%,相对标准偏差为3%～8%。12地最终残留试验表明,50%吡蚜酮水分散粒剂按有效成分225 g/hm²施药2次,最后1次施药后14、21 d马铃薯中吡蚜酮残留量分别≤0.018 mg/kg和≤0.012 mg/kg。膳食风险评估表明,吡蚜酮的国家估算每日摄入量(NEDI)为1.633 9 mg/kg,风险商(RQ)为86.4%。马铃薯中吡蚜酮残留不会对一般人群健康造成不可接受的风险。     

超高效液相色谱-串联质谱法测定柑橘中的草甘膦及其代谢物残留

本研究首次建立了一种超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定柑橘中草甘膦及其代谢物N-乙酰草甘膦?氨甲基磷酸(AMPA)和N-乙酰AMPA?样品经过0.5%甲酸水提取, 以十八烷基硅烷键合硅胶柱(C18)净化, 利用水和200 mmol/L碳酸氢铵溶液(含0.1%氨水)作为流动相梯度洗脱, 在多反应监测模式下定量分析?结果表明, 草甘膦及其代谢物在0.05~1 mg/kg范围内线性关系良好, 相关系数均大于0.99; 草甘膦及其3个代谢物在柑橘全果和果肉基质中3个加标水平下回收率为 70.5%~109.5%, 相对标准偏差(RSD)为0.6%~10.1%, 定量限为0.05 mg/kg?本方法的前处理样品无需衍生, 简便?快捷?高效?准确可靠, 可用于柑橘中草甘膦及其代谢物N-乙酰草甘膦?AMPA和N-乙酰AMPA的定量检测?     

四种替代药剂对梨火疫病菌的抑制活性及其田间防效

为筛选农用链霉素替代药剂,以其为对照药剂,测定春雷霉素、中生菌素、噻霉酮和噻菌铜这4种常用细菌病害防治药剂对梨火疫病菌Erwinia amylovora的抑制活性、对梨火疫病的田间防效及不同药剂处理后梨中的农药残留,并对这4种药剂的作物安全性进行评价。结果表明,中生菌素、噻霉酮和春雷霉素对梨火疫病菌有抑制作用,抑制中浓度EC50分别为1.60、6.64和60.57 mg/L,中生菌素的抑制效果高于链霉素。在连续2年田间试验中,中生菌素1 000倍液和春雷霉素400倍液对梨火疫病的保护效果和治疗效果均达90.33%以上,噻霉酮500倍液和噻菌铜200倍液对梨火疫病的保护效果均达100.00%,治疗效果均超过86.97%,与对照药剂农用链霉素2 000倍液的效果相当。所有药剂处理后均未检出中生菌素、春雷霉素、高效氯氰菊酯和农用链霉素的农药残留,而噻虫嗪、阿维菌素和矮壮素虽有检出,但其残留量均低于国家限量标准。花期前后、幼果期和果实膨大期施药,中生菌素、春雷霉素、噻霉酮和噻菌铜对梨花、叶片、枝梢及果实生长均无不良影响。综合来看,中生菌素、春雷霉素、噻霉酮和噻菌铜均可作为农用链霉素的替代药剂,...     

Study on Feed Value of Cassava Residue for Growing-Fishing Pigs

To determine the apparent digestibility of cassava residue (CR) nutrient and the effects of CR on growth performance when replaced the different levels corn in diet,two experiments were designed.In the first experiment,8 Duroc×Landrace×Yorkshire crossbred barrow pigs with the similar weight (22.46 kg±1.08 kg) were chosen for determining the apparent digestibility of CR.The pre-test period lasted for 10 days,and the trial period lasted for 5 days.In the second experiment,160 Duroc×Landrace×Yorkshire crossbred pigs with the similar weight(21.09 kg±0.72 kg) were randomly divided into five groups with four replicates per group and eight pigs per replicate.The control group was fed with basal diet while the experimental groups were fed diets containing 5%,10%,15% and 20% levels of substitution of corn by CR,respectively.The pre-test period lasted for 5 days,and the trial period lasted for 30 days.The results showed that the content of CP and EE in CR were 2.73% and 0.68%,but CF and total energy were 15.34% and 13.55 MJ/kg.The content of Lys and Thr were 0.11% and 0.08%,respectively.Calcium and phosphorus apparent digestibility were low,just only 40.24% and 34.76%,respectively,while apparent total energy digestibility was 65.62%.The apparent digestibility of Arg,Glu,Tyr,Met,Leu and Val were higher than 80%.The average daily gain was reduced with increasing dose of CR,which the group of 15% and 20% addition were significantly lower than that of control group (P< 0.05).However,the average daily gain of 5% and 10% groups were no significant difference with the control group(P >0.05).The feed cost of 5% and 10% addition groups were decreased by 0.01 and 0.05 yuan.In conclusion,under this experimental condition,the appropriate addition of CR for growing-fishing pig (20 to 50 kg ) was 5% to 10% in the diet.     

LC-MS/MS measurement of ampicillin residue in swine tissues at 5 days after in-feed administration

We assessed ampicillin (ABPC) concentrations of kidney, muscle and intestine after a 5–day withdrawal period in 2 male and a female young Large White pigs fed the diet containing ABPC (ABPC medicated feed, 24 mg/kg/day) for a week. The ABPC residues were measured with liquid chromatography–tandem mass spectrometry, and the mean recoveries and quantitation limits ranged from 91.8 to 97.2% and from 0.1 to 0.12 ng/g, respectively. The residual ABPC concentrations were ≤1.18 ng/g for the muscle, ≤0.53 ng/g for the kidney and ≤1.93 ng/g for the intestine, suggesting below the Japanese provisional maximum residue limits. These results reveal that the analytical method is developed for residual ABPC and that the withdrawal period is appropriate.     

动物源食品中酰胺醇类药物及其代谢物残留检测超高效液相色谱-串联质谱法研究

建立了动物源食品中酰胺醇类药物(氯霉素CAP、甲砜霉素TAP、氟苯尼考FF)及其代谢物(氟苯尼考胺FFA)残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)法。样品经氨化乙酸乙酯提取,正已烷脱脂,氨化乙酸乙酯反萃取,电喷雾正/负离子多反应监测(MRM)模式检测。四种药物在0.2~50μg/L的系列浓度范围呈线性相关,样品中CAP的检测限为0.1μg/kg,定量限为0.2μg/kg;TAP、FF、FFA检测限为0.5μg/kg,定量限为1.0μg/kg。在0.2~5μg/kg的添加浓度范围内平均回收均为80%~120%,变异系数均小于15%。结果表明该方法简单快速、灵敏度高、重复性好,适用于动物源食品中酰胺醇类及其代谢物残留检测。     

中药药渣利用方法研究现状及高值化利用思考

随着中医行业发展和中医药制取技术的进步,中药渣的产生也与日俱增,现年产量已超过3500万吨。利用好中药渣资源不仅能保护环境,降低企业支出,还能创造额外的巨大经济效益。本文总结了中药渣在活性成分再提取、环境治理、作为饲料或饲料添加剂、作为有机肥料与栽培基质、作为轻工业生产原料等传统生态经济化利用现状,以及开发能源物质、膳食纤维产品、纳米纤维素类产品及复合材料等高值化利用现状,以期为中医药产业实现高质量发展提供参考。