有效的净化方式是获取兽药多残留高质量分析结果的重要前提。本文建立了Oasis PRiME HLB净化后经液质联用同时测定动物源性食品中β-受体激动剂类、喹诺酮类、磺胺类、氯霉素类、大环内酯类、镇静剂类、硝基咪唑类、阿维菌素类、抗病毒...有效的净化方式是获取兽药多残留高质量分析结果的重要前提。本文建立了Oasis PRiME HLB净化后经液质联用同时测定动物源性食品中β-受体激动剂类、喹诺酮类、磺胺类、氯霉素类、大环内酯类、镇静剂类、硝基咪唑类、阿维菌素类、抗病毒类、四环素类、非甾体类、青霉素类、头孢类物质的兽药多残留检测方法。试样用含0.2%甲酸的80%乙腈水提取及Oasis PRiME HLB净化后,经InfinityLab Poroshell 120 EC-C18色谱柱分离,三重四极杆液质联用系统检测。结果表明,13大类69种兽药残留在0.1~50 ng/mL浓度范围内线性关系良好(R2≥0.99),基质匹配或内标法定量的回收率为84.2%~113%,相对标准偏差均<8.9%。展开更多
建立了超高效液相色谱串联质谱法同时测定56种动物源性兽药残留物的分析方法。以乙腈-0.5%乙酸水溶液(85:15,V/V)为提取溶剂,采用固相萃取柱(Oasis PRi ME HLB)进行样品净化,通过UPLC-MS/MS分析测定,基质曲线外标法定量。方法定量限为1....建立了超高效液相色谱串联质谱法同时测定56种动物源性兽药残留物的分析方法。以乙腈-0.5%乙酸水溶液(85:15,V/V)为提取溶剂,采用固相萃取柱(Oasis PRi ME HLB)进行样品净化,通过UPLC-MS/MS分析测定,基质曲线外标法定量。方法定量限为1.0μg/kg(喹诺酮类)、1.5μg/kg(糖皮质类)、10μg/kg(磺胺类)、1.0μg/kg(β-受体激动剂类)。56种兽药残留物在牛肉、猪肉、鸡肉和奶等基质样品中回收率范围为63.2%~101.5%,基质标准工作曲线线性相关系数大于0.937,精密度RSD<15%(n=3)。方法适用于动物源性食品中兽药残留物的分析。展开更多
目的建立高效液相色谱串联质谱法快速检测鸡蛋中硝基咪唑类药物残留量的分析方法。方法以0.1%甲酸乙腈为提取溶剂,加入盐析剂分层后,用Waters Oasis PRiME HLB法净化,用乙腈和0.1%(V:V)甲酸水溶液作为流动相进行梯度洗脱, C18色谱柱分离...目的建立高效液相色谱串联质谱法快速检测鸡蛋中硝基咪唑类药物残留量的分析方法。方法以0.1%甲酸乙腈为提取溶剂,加入盐析剂分层后,用Waters Oasis PRiME HLB法净化,用乙腈和0.1%(V:V)甲酸水溶液作为流动相进行梯度洗脱, C18色谱柱分离,在高效液相色谱-串联质谱仪上采用电喷雾正离子扫描模式检测,基质匹配标准曲线外标法定量。结果该方法在0.5~100 ng/mL范围内具有良好线性关系, 10种硝基咪唑类药物相关系数均大于(r^2)>0.99,方法检出限在0.1~0.3μg/kg范围,定量限在0.3~0.5μg/kg范围。3个浓度水平1.0、5.0、10.0μg/kg加标,平均回收率分别为82.5%~119.1%、80.7%~112.3%、80.6%~118.5%,相对标准偏差(relative standard deviation, RSD)为1.2%~9.1%。结论该方法具有快速、简便、准确、灵敏的特点,适用于鸡蛋中硝基咪唑残留量的分析检测,可用于日常大批量快速筛查工作,有效提高日常工作效率。展开更多
The Asiatic citrus psyllid （Diaphorina cirri Kuwayama [Hemiptera： Sternorrhyncha： Psyllidae] is a vector ofhuanglongbing （citrus greening）, a devastating disease of citrus caused by phloem-limited bacteria. Growi...The Asiatic citrus psyllid （Diaphorina cirri Kuwayama [Hemiptera： Sternorrhyncha： Psyllidae] is a vector ofhuanglongbing （citrus greening）, a devastating disease of citrus caused by phloem-limited bacteria. Growing guava （Psidium guajava） as an intercrop appears to be a successful means of reducing psyllid numbers within citrus orchards; however, the mechanism by which such a reduction is achieved is unknown. To determine the repellent effect of guava leaf and factors attributed to this activity, responses of adult psyllids to guava leaf and its odor were evaluated in cage tests and Y-tube olfactometer test. The results showed that guava leaf possessed a repellent effect against the adult citrus psyllids. Fewer psyllids were found on citrus leaves in the presence of guava foliage than in its absence. Young and old guava leaf showed equal repellent activity. By covering the guava shoots with net cloth, it was revealed that the repellent effect of guava leaf against adult psyllids on citrus was attributed to the volatile compounds, rather than physical factors. The olfactometer response of adult psyllids to guava leaf odor was dosage-dependent. Between guava odor and control, only 35.00%, 25.00% and 16.25% of the psyllids moved toward guava odor when presented with 5.0, 10.0 and 15.0 g of guava shoots, respectively. The olfactometer experiments also showed that both male and female psyllids responded similarly to the guava leaf odor.展开更多
目的建立PRiMEHLB固相萃取柱结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)快速测定茶叶中200种农药残留量的分析方法。方法样品用乙腈提取,经PRiME HLB通过式固相萃取柱净化,残留量采用气相色谱-串...目的建立PRiMEHLB固相萃取柱结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)快速测定茶叶中200种农药残留量的分析方法。方法样品用乙腈提取,经PRiME HLB通过式固相萃取柱净化,残留量采用气相色谱-串联质谱法进行检测。结果200种农药在各自质量浓度范围内均呈现良好线性关系,相关系数(r^(2))均大于等于0.995,方法定量限在0.01~0.05mg/kg之间。在阴性茶叶中加入低、中、高3个添加水平,平均加标回收率及相对标准偏差分别为70.0%~129.2%、1.0%~23.7%。结论该方法操作便捷、快速、准确性强,适合于茶叶中农药多残留高通量的筛查。展开更多
文摘为实现柑橘黄龙病的早期、快速确诊,有效阻止病害蔓延,达到早期防治、保障柑橘生产的目的,该文研究基于高光谱成像的柑橘黄龙病早期无损检测及病情分级,并对多种预处理方法的建模结果进行探讨。试验获取370～1 000 nm健康、不同染病程度及缺锌共5类柑橘叶片的高光谱图像,用遥感图像处理平台(environment for visualizing images,ENVI)得到各类样本感兴趣区域的光谱反射率平均值。运用一阶微分、移动窗口拟和多项式平滑(savitzky-golay,SG)进行数据处理,结合偏最小二乘判别分析(partial least squares-discriminate analysis,PLS-DA)构建黄龙病的早期鉴别及病情分级模型。结果表明:建立的3个判别模型,验证集相关系数均不低于0.9548。其中,经SG平滑及一阶微分预处理所建立的模型分类效果最佳,总体预测准确率达96.4%,预测均方根误差0.1344。该研究为柑橘病害早期诊断和预警提供了新方法,也为黄龙病病害程度遥感监测提供了基础。
文摘有效的净化方式是获取兽药多残留高质量分析结果的重要前提。本文建立了Oasis PRiME HLB净化后经液质联用同时测定动物源性食品中β-受体激动剂类、喹诺酮类、磺胺类、氯霉素类、大环内酯类、镇静剂类、硝基咪唑类、阿维菌素类、抗病毒类、四环素类、非甾体类、青霉素类、头孢类物质的兽药多残留检测方法。试样用含0.2%甲酸的80%乙腈水提取及Oasis PRiME HLB净化后,经InfinityLab Poroshell 120 EC-C18色谱柱分离,三重四极杆液质联用系统检测。结果表明,13大类69种兽药残留在0.1~50 ng/mL浓度范围内线性关系良好(R2≥0.99),基质匹配或内标法定量的回收率为84.2%~113%,相对标准偏差均<8.9%。
文摘建立了超高效液相色谱串联质谱法同时测定56种动物源性兽药残留物的分析方法。以乙腈-0.5%乙酸水溶液(85:15,V/V)为提取溶剂,采用固相萃取柱(Oasis PRi ME HLB)进行样品净化,通过UPLC-MS/MS分析测定,基质曲线外标法定量。方法定量限为1.0μg/kg(喹诺酮类)、1.5μg/kg(糖皮质类)、10μg/kg(磺胺类)、1.0μg/kg(β-受体激动剂类)。56种兽药残留物在牛肉、猪肉、鸡肉和奶等基质样品中回收率范围为63.2%~101.5%,基质标准工作曲线线性相关系数大于0.937,精密度RSD<15%(n=3)。方法适用于动物源性食品中兽药残留物的分析。
文摘目的建立高效液相色谱串联质谱法快速检测鸡蛋中硝基咪唑类药物残留量的分析方法。方法以0.1%甲酸乙腈为提取溶剂,加入盐析剂分层后,用Waters Oasis PRiME HLB法净化,用乙腈和0.1%(V:V)甲酸水溶液作为流动相进行梯度洗脱, C18色谱柱分离,在高效液相色谱-串联质谱仪上采用电喷雾正离子扫描模式检测,基质匹配标准曲线外标法定量。结果该方法在0.5~100 ng/mL范围内具有良好线性关系, 10种硝基咪唑类药物相关系数均大于(r^2)>0.99,方法检出限在0.1~0.3μg/kg范围,定量限在0.3~0.5μg/kg范围。3个浓度水平1.0、5.0、10.0μg/kg加标,平均回收率分别为82.5%~119.1%、80.7%~112.3%、80.6%~118.5%,相对标准偏差(relative standard deviation, RSD)为1.2%~9.1%。结论该方法具有快速、简便、准确、灵敏的特点,适用于鸡蛋中硝基咪唑残留量的分析检测,可用于日常大批量快速筛查工作,有效提高日常工作效率。
基金Our research was supported by special funds from the National Science Foundation of China （30471169）, the President＇s Foundation of South China Agricultural University （2007G003）, and the Department of Education, Science and Training of the Commonwealth of Australia （CH060068）. We thank Dr. Yi-Jing Cen and Mr. Ke- Cheng Huang for their kind cooperation during the study.
文摘The Asiatic citrus psyllid （Diaphorina cirri Kuwayama [Hemiptera： Sternorrhyncha： Psyllidae] is a vector ofhuanglongbing （citrus greening）, a devastating disease of citrus caused by phloem-limited bacteria. Growing guava （Psidium guajava） as an intercrop appears to be a successful means of reducing psyllid numbers within citrus orchards; however, the mechanism by which such a reduction is achieved is unknown. To determine the repellent effect of guava leaf and factors attributed to this activity, responses of adult psyllids to guava leaf and its odor were evaluated in cage tests and Y-tube olfactometer test. The results showed that guava leaf possessed a repellent effect against the adult citrus psyllids. Fewer psyllids were found on citrus leaves in the presence of guava foliage than in its absence. Young and old guava leaf showed equal repellent activity. By covering the guava shoots with net cloth, it was revealed that the repellent effect of guava leaf against adult psyllids on citrus was attributed to the volatile compounds, rather than physical factors. The olfactometer response of adult psyllids to guava leaf odor was dosage-dependent. Between guava odor and control, only 35.00%, 25.00% and 16.25% of the psyllids moved toward guava odor when presented with 5.0, 10.0 and 15.0 g of guava shoots, respectively. The olfactometer experiments also showed that both male and female psyllids responded similarly to the guava leaf odor.
文摘目的建立PRiMEHLB固相萃取柱结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)快速测定茶叶中200种农药残留量的分析方法。方法样品用乙腈提取,经PRiME HLB通过式固相萃取柱净化,残留量采用气相色谱-串联质谱法进行检测。结果200种农药在各自质量浓度范围内均呈现良好线性关系,相关系数(r^(2))均大于等于0.995,方法定量限在0.01~0.05mg/kg之间。在阴性茶叶中加入低、中、高3个添加水平,平均加标回收率及相对标准偏差分别为70.0%~129.2%、1.0%~23.7%。结论该方法操作便捷、快速、准确性强,适合于茶叶中农药多残留高通量的筛查。
