液相色谱-串联质谱法测定猪尿液中地西泮及其7种代谢物残留

为建立快速测定猪尿中地西泮及其7种代谢物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)确证方法,本研究优化了样品净化的阳离子交换固相萃取柱(PCX柱)及其淋洗洗脱条件。猪尿液酸化后直接经PCX柱净化,依次用水、60%甲醇水溶液淋洗,最后用5%氨化甲醇洗脱;选用BEH C18色谱柱分离,UPLCMS/MS进行检测,以基质匹配标准曲线定量。结果显示:8种药物在0.3~20.0μg/L范围内具有良好的线性关系(R²≥0.995),检出限和定量限分别为0.1μg/L和0.3μg/L;各药物在3个添加浓度下回收率为73.6%~95.3%,日内、日间相对标准偏差分别为2.9%~18.6%(n=6)和2.2%~12.6%(n=3)。结果表明,本方法操作简单、快速,灵敏度高、特异性好。     

凉茶渣的黑曲霉发酵工艺和抗氧化活性研究

为促进凉茶渣在畜牧业中的资源化利用,本研究以黑曲霉为菌种固态发酵凉茶渣,首先在单因素试验条件下考察了时间、温度、含水量、浸泡液pH、氮源和碳源对凉茶渣降解率和产物pH的影响;再根据单因素试验结果和规模化生产实际需要,以4%硫酸铵为氮源,2%葡萄糖为碳源,以降解率为考察指标,通过正交试验优化发酵工艺;并通过检测超氧自由基清除率、羟基自由基清除率和1,1-二苯基-2-三硝基苯肼（DPPH）自由基清除率,评价凉茶渣在最优工艺条件下发酵前后抗氧化活性的变化。结果发现,含水量为60%,浸泡液pH为9.0,31℃发酵168 h是凉茶渣的最佳发酵工艺参数。最佳工艺条件下凉茶渣的降解率为25.23%,发酵产物pH为4.53。当凉茶渣发酵前水提液浓度为24 mg/mL时,超氧自由基清除率为43.56%,羟基自由基清除率为47.06%,DPPH自由基清除率为90.71%;当最优条件下发酵产物水提液浓度24 mg/mL时,超氧自由基清除率为30.77%,羟基自由基清除率为95.63%,DPPH自由基清除率为87.36%。本试验结果表明,黑曲霉是适宜的凉茶渣发酵菌种,且凉茶渣经过黑曲霉发酵后具有良好的抗氧化活性。     

木薯渣发酵饲料及其发酵工艺与应用

文章旨在研究木薯渣发酵饲料及其发酵工艺与应用。将木薯渣、玉米面、豆粕、玉米皮、麸皮按照质量比50∶5∶10∶10∶25的比例混合,然后将乳酸菌和酵母菌按比例与一定量的水混合,再与木薯渣饲料混匀,装入带有呼吸阀的发酵袋中,密封,室温条件下发酵4 d即生产得到木薯渣发酵饲料。结果表明：乳酸菌和酵母菌混合比例为1∶2,接种量为0.1%,水分为40%～45%时,木薯渣发酵饲料pH<4.5,酸溶蛋白和总酸含量明显增加,具有明显的酸香气味,可提高适口性;可抑制霉菌生长,确保产品安全性;还可提高饲料的营养水平和猪只消化率,提高饲料利用率;提高猪只生产性能,降低圈舍氨气浓度,改善舍内环境;同时还为木薯渣资源化利用提供良好的前提条件。     

Residue Detection of Tetracyclines in Eggs by High Performance Liquid Chromatography

The study was aimed to establish the method of simultaneous detection of four kinds of tetracyclines,including oxytraoycline,tetracycline,chlortetracycline and doxyeycline in eggs by high performance liquid chromatography (HPLC).The eggs samples were detected with HPLC after through the procedure of extraction of 0.1 mol/L Na₂EDTA-Mcllvaine buffered solution,purification of Oasis MAX solid-phase extraction column,gradient elution of taking acetonitrile-0.01 mol/mL trifluoroacetic acid as mobile phase,separation with reverse liquid chromatography.The results showed that the calibration curves of four kinds of tetracyclines were linear correlated in the concentration range of 30 to 1 000 ng/g which the limits of detection was 10 ng/g and the limit of quantification was 50 ng/g.The average recoveries were 67.3% to 81.4%,relative standard deviations of intraday was 2.7% to 14.3%,relative standard deviations of inter-day was 0.9% to 5.0%.This mothod established in this study could simultaneously detect oxytetracycline,tetracycline,chlortetracycline and doxycycline drug residues in egg and it had high sensitivity,accuracy and precision.The method was rapid and simple to operate.     

Growth performance,carcass traits,physiochemical characteristics and intramuscular fatty acid composition of finishing Japanese black steers fed soybean curd residue and soy sauce cake

This study was conducted to determine the effects of dietary soybean curd residue (SCR) and soy sauce cake (SSC) on the growth performance, carcass traits and physiochemical and intramuscular fatty acid (FA) characteristics in Japanese Black steers. Ten steers (29.7 ± 0.3 months old, 856.6 ± 24.4 kg body weight) were assigned to either treatment C, fed a conventional concentrate or T, fed the test diet including dried SCR and SSC for 3 months. In growth performance, dry matter (DM) intake and average daily gain, and carcass traits did not differ significantly between the treatments. Color of beef was affected by the dietary treatments and meat samples from T showed higher a^* value and chroma than those in C. On FA composition, there was no significant difference between the treatments in neutral lipids, whereas in polar lipids, meat samples from T had higher C16:1 (P < 0.05) and tended to have higher C16:0 (P = 0.05) and C18:1 (P = 0.08), but lower C17:0 (P = 0.098), C18:2 (P = 0.06) and C20:4 (P = 0.07) than those from C. The study suggested that SCR and SSC could be used as a substitute for conventional concentrate and would influence meat color and intramuscular FA composition of polar lipids.     

丹参药渣栽培糙皮侧耳和毛头鬼伞

采用不同比例丹参(Salviae miltiorrhiza)药渣替代玉米芯对糙皮侧耳(Pleurotus ostreatus)、毛头鬼伞(Coprinus comatus)供试菌株进行栽培实验.经栽培收获两茬子实体,分别对不同配方两个菌种的菌丝长速、单位料重产量、生物学效率等指标进行统计分析.结果表明:在单位料重产量及生物学效率表现上,随培养料中所含丹参药渣比例增加而增加;在菌丝长速表现上则相反.经丹参药渣、玉米芯的碳氮比分析(28.5∶1;88.1∶1)得知,栽培料中随药渣含量的增加氮素含量相应提高(碳氮比55.27∶1～27.44∶1,氮含量为0.76％～2.43％),成为两个菌种产量增加的主要原因.     

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。     

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.     

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?