Pesticide residue analysis plays an important role in the quality control of Chinese materia medica.This paper reports the development and validation of an analytical method for the quantitative determination of the r...Pesticide residue analysis plays an important role in the quality control of Chinese materia medica.This paper reports the development and validation of an analytical method for the quantitative determination of the residues of 39 pesticides in 12 different matrices of Chinese materia medica.Sample preparation utilized the QuEChERS method with acetonitrile:1% aqueous acetic acid(9:1,v/v)as extraction solvent followed by sample clean-up by dispersive solid phase extraction using primary secondary amine sorbent and graphitized carbon black.Extracts were then analysed by gas chromatography coupled with electron impact mass spectrometry in the selected ion monitoring mode.Limit of detection(LOD)and limit of quantitation(LOQ)values were in the ranges 0.5-50 ng/g and 1-100 ng/g,respectively.The recoveries of the 39 pesticides were in the range 75-112% with precision(as relative standard deviation,RSD)<15%.The results show that the modified QuEChERS method allows rapid and sensitive analysis of multiple pesticide residues in Chinese materia medica.展开更多
The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction （USE） and their chemical constituents were analyzed by gas chromatographymass spectrometry （GC-MS） to provide s...The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction （USE） and their chemical constituents were analyzed by gas chromatographymass spectrometry （GC-MS） to provide scientific basis for the quality control of safflower. Five different solvents （diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone） were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC-MS is a simple, rapid and effective method to analyze the volatile oil components of safflower.展开更多
基金This work was supported by a project grant(No.09ZZ008)from the Scientific Research Fund of Sichuan Provincial Education Department,China.
文摘Pesticide residue analysis plays an important role in the quality control of Chinese materia medica.This paper reports the development and validation of an analytical method for the quantitative determination of the residues of 39 pesticides in 12 different matrices of Chinese materia medica.Sample preparation utilized the QuEChERS method with acetonitrile:1% aqueous acetic acid(9:1,v/v)as extraction solvent followed by sample clean-up by dispersive solid phase extraction using primary secondary amine sorbent and graphitized carbon black.Extracts were then analysed by gas chromatography coupled with electron impact mass spectrometry in the selected ion monitoring mode.Limit of detection(LOD)and limit of quantitation(LOQ)values were in the ranges 0.5-50 ng/g and 1-100 ng/g,respectively.The recoveries of the 39 pesticides were in the range 75-112% with precision(as relative standard deviation,RSD)<15%.The results show that the modified QuEChERS method allows rapid and sensitive analysis of multiple pesticide residues in Chinese materia medica.
文摘The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction （USE） and their chemical constituents were analyzed by gas chromatographymass spectrometry （GC-MS） to provide scientific basis for the quality control of safflower. Five different solvents （diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone） were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC-MS is a simple, rapid and effective method to analyze the volatile oil components of safflower.
