[Objectives]The paper was to establish an ultra high performance liquid chromatography-quadrupole/linear ion trap complex mass spectrometry for the determination of 10 kinds ofα2-receptor agonists in animal derived f...[Objectives]The paper was to establish an ultra high performance liquid chromatography-quadrupole/linear ion trap complex mass spectrometry for the determination of 10 kinds ofα2-receptor agonists in animal derived food.[Methods]The samples were extracted with sodium carbonate buffer solution and ethyl acetate,and analyzed by mass spectrometry after solid phase extraction and high performance liquid chromatography separation.[Results]Ten kinds ofα2-receptor agonists showed a good linear relationship in the range of 1-100μg/mL,with the average recovery of over 69%and the relative standard deviation less than 8.32%.The detection limit of 10 kinds of α_(2)-receptor agonists was up to 1μg/kg.[Conclusions]The method has good selectivity and strong anti-interference ability,and can meet the requirements of 10 kinds ofα2-receptor agonists residues in animal derived food.展开更多
Suppressing effects of mass trapping using synthetic sex pheromone with main active ingredients of Z-11-hexadecenal, Z-13-octadecenal and Z-9-hexadecenal on the rice stem borer, Chilo suppressalis were investigated du...Suppressing effects of mass trapping using synthetic sex pheromone with main active ingredients of Z-11-hexadecenal, Z-13-octadecenal and Z-9-hexadecenal on the rice stem borer, Chilo suppressalis were investigated during the flight periods of the overwintering and 1st generation in the paddy area of 60 ha in 1999. Population density of C. suppressalis in the pheromone-treated fields was lower than that in control. The egg masses decreased by 74.39% and population size of adult males of the 1st generation decreased by 61.64% in the treated fields as compared to control. Meanwhile, the damage by C. suppressalis larvae was significantly lower in the treated fields than control (t-test, P=0.05). Percentages of brownish leaf sheath, dead heart, and white head in the treated fields were decreased by 70.90%, 57.01% and 44.30%, respectively in contrast to control. The present study demonstrated that mass trapping to C. suppressalis using synthetic sex pheromone shows great potential as an alternative measure in an environment-friendly pest management and at the same challenging the insecticide use that has some environment impacts.展开更多
In this study,we established a comprehensive method for simultaneous identification and quantification of tetrodotoxin(TTX) in fresh pufferfish tissues and pufferfish-based products using liquid chromatography/quadrup...In this study,we established a comprehensive method for simultaneous identification and quantification of tetrodotoxin(TTX) in fresh pufferfish tissues and pufferfish-based products using liquid chromatography/quadrupole-linear ion trap mass spectrometry(LC-QqLIT-MS).TTX was extracted by 1% acetic acid-methanol,and most of the lipids were then removed by freezing lipid precipitation,followed by purification and concentration using irnmunoaffinity columns(IACs).Matrix effects were substantially reduced due to the high specificity of the IACs,and thus,background interference was avoided.Quantitation analysis was therefore performed using an external calibration curve with standards prepared in mobile phase.The method was evaluated by fortifying samples at 1,10,and 100 ng/g,respectively,and the recoveries ranged from 75.8%-107%,with a relative standard deviation of less than 15%.The TTX calibration curves were linear over the range of 1-1 000 ng/L,with a detection limit of 0.3 ng/g and a quantification limit of 1 ng/g.Using this method,samples can be further analyzed using an informationdependent acquisition(IDA) experiment,in the positive mode,from a single liquid chromatography-tandem mass spectrometry injection,which can provide an extra level of confirmation by matching the full product ion spectra acquired for a standard sample with those from an enhanced product ion(EPI) library.The scheduled multiple reaction monitoring method enabled TTX to be screened for,and TTX was positively identified using the IDA and EPI spectra.This method was successfully applied to analyze a total of 206 samples of fresh pufferfish tissues and pufferfish-based products.The results from this study show that the proposed method can be used to quantify and identify TTX in a single run with excellent sensitivity and reproducibility,and is suitable for the analysis of complex matrix pufferfish samples.展开更多
基金Supported by Scientific Research Project of Dalian Customs(2022DK09).
文摘[Objectives]The paper was to establish an ultra high performance liquid chromatography-quadrupole/linear ion trap complex mass spectrometry for the determination of 10 kinds ofα2-receptor agonists in animal derived food.[Methods]The samples were extracted with sodium carbonate buffer solution and ethyl acetate,and analyzed by mass spectrometry after solid phase extraction and high performance liquid chromatography separation.[Results]Ten kinds ofα2-receptor agonists showed a good linear relationship in the range of 1-100μg/mL,with the average recovery of over 69%and the relative standard deviation less than 8.32%.The detection limit of 10 kinds of α_(2)-receptor agonists was up to 1μg/kg.[Conclusions]The method has good selectivity and strong anti-interference ability,and can meet the requirements of 10 kinds ofα2-receptor agonists residues in animal derived food.
文摘Suppressing effects of mass trapping using synthetic sex pheromone with main active ingredients of Z-11-hexadecenal, Z-13-octadecenal and Z-9-hexadecenal on the rice stem borer, Chilo suppressalis were investigated during the flight periods of the overwintering and 1st generation in the paddy area of 60 ha in 1999. Population density of C. suppressalis in the pheromone-treated fields was lower than that in control. The egg masses decreased by 74.39% and population size of adult males of the 1st generation decreased by 61.64% in the treated fields as compared to control. Meanwhile, the damage by C. suppressalis larvae was significantly lower in the treated fields than control (t-test, P=0.05). Percentages of brownish leaf sheath, dead heart, and white head in the treated fields were decreased by 70.90%, 57.01% and 44.30%, respectively in contrast to control. The present study demonstrated that mass trapping to C. suppressalis using synthetic sex pheromone shows great potential as an alternative measure in an environment-friendly pest management and at the same challenging the insecticide use that has some environment impacts.
基金Supported by the National Natural Science Foundation of China(No.41106109)the China National Food Safety Standards Development Project(No.ZHENGHE-2015-356)
文摘In this study,we established a comprehensive method for simultaneous identification and quantification of tetrodotoxin(TTX) in fresh pufferfish tissues and pufferfish-based products using liquid chromatography/quadrupole-linear ion trap mass spectrometry(LC-QqLIT-MS).TTX was extracted by 1% acetic acid-methanol,and most of the lipids were then removed by freezing lipid precipitation,followed by purification and concentration using irnmunoaffinity columns(IACs).Matrix effects were substantially reduced due to the high specificity of the IACs,and thus,background interference was avoided.Quantitation analysis was therefore performed using an external calibration curve with standards prepared in mobile phase.The method was evaluated by fortifying samples at 1,10,and 100 ng/g,respectively,and the recoveries ranged from 75.8%-107%,with a relative standard deviation of less than 15%.The TTX calibration curves were linear over the range of 1-1 000 ng/L,with a detection limit of 0.3 ng/g and a quantification limit of 1 ng/g.Using this method,samples can be further analyzed using an informationdependent acquisition(IDA) experiment,in the positive mode,from a single liquid chromatography-tandem mass spectrometry injection,which can provide an extra level of confirmation by matching the full product ion spectra acquired for a standard sample with those from an enhanced product ion(EPI) library.The scheduled multiple reaction monitoring method enabled TTX to be screened for,and TTX was positively identified using the IDA and EPI spectra.This method was successfully applied to analyze a total of 206 samples of fresh pufferfish tissues and pufferfish-based products.The results from this study show that the proposed method can be used to quantify and identify TTX in a single run with excellent sensitivity and reproducibility,and is suitable for the analysis of complex matrix pufferfish samples.
