Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS col...Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.展开更多
[Objective] This study aimed to establish a determination method for iprobenfos residue in rice straw and husked rice. [Method] The rice straw and husked rice samples were extracted by acetone-ethyl acetate mixed solv...[Objective] This study aimed to establish a determination method for iprobenfos residue in rice straw and husked rice. [Method] The rice straw and husked rice samples were extracted by acetone-ethyl acetate mixed solvent. The extracts were purified using SPE C18 column and SPE NH2 column, and the iprobenfos residues were determined by GC-FTD. [Result] In the concentration range of 0.005-5.0 mg/kg, iprobenfos concentration showed a good linear relationship with peak area （r=0.999 8）. When the iprobenfos concentrations were 0.01, 0.1 and 1.0 mg/kg respectively, the recoveries of added iprobenfos from rice straw ranged from 72.6% to 99.7% with relative standard deviation ranging from 5.65% to 8.48%; the recoveries of added iprobenfos from husked rice ranged from 81.6% to 97.6% with relative standard deviation ranging from 3.74% to 7.63%. The minimum detectable quantity of iprobenfos was 5×10^-12 g, and the minimum detectable concentrations of iprobenfos in rice straw and husked rice samples were 2.0 and 0.5 μg/kg, respec- tively. [Conclusion] The established determination method is characterized by low de- termination limit, high sensitivity, good reproducibility and high operability, which all meet the requirements by Guideline on Pesticide Residue Trials of the Ministry of Agriculture.展开更多
Forty-eight vinegar samples including white vinegar, rice vinegar and mature vinegar were collected from several markets in Beijing. Butyltin compounds were determined by headspace solid-phase microextraction coupled ...Forty-eight vinegar samples including white vinegar, rice vinegar and mature vinegar were collected from several markets in Beijing. Butyltin compounds were determined by headspace solid-phase microextraction coupled with gas chromatography and flame photometric detector after in situ ethylation with sodium tetraethylborate. Butyltin species were detected in sixteen vinegar samples and ranged from 0.012 to 14.10 lag Sn L 1. The detection rate of white vinegar is higher than that of rice vinegar and mature vinegar. Vinegar samples with relatively high butyltin concentration (〉1.5 μg Sn L-1) were those stored in plastic bags, indicating that the plastic bag was one of the possible sources of butyltin contamination. This was further confirmed by the leaching experiments of three selected plastic bags, and monobutyltin was detected in the leaching solvents. According to the estimation, the average daily intake of total butyltin compounds through vinegar consumption is about 0.04 ng Sn/kg b.w., much lower than the Tolerable Daily Intake (TDI) of 100 ng Sn/kg b.w. set by the European Food Safety Authority (EFSA).展开更多
文摘Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.
基金Supported by Pesticide Registration Residual Test of Institute for the Control of Agrochemicals,Ministry of Agriculture(2013F216)~~
文摘[Objective] This study aimed to establish a determination method for iprobenfos residue in rice straw and husked rice. [Method] The rice straw and husked rice samples were extracted by acetone-ethyl acetate mixed solvent. The extracts were purified using SPE C18 column and SPE NH2 column, and the iprobenfos residues were determined by GC-FTD. [Result] In the concentration range of 0.005-5.0 mg/kg, iprobenfos concentration showed a good linear relationship with peak area （r=0.999 8）. When the iprobenfos concentrations were 0.01, 0.1 and 1.0 mg/kg respectively, the recoveries of added iprobenfos from rice straw ranged from 72.6% to 99.7% with relative standard deviation ranging from 5.65% to 8.48%; the recoveries of added iprobenfos from husked rice ranged from 81.6% to 97.6% with relative standard deviation ranging from 3.74% to 7.63%. The minimum detectable quantity of iprobenfos was 5×10^-12 g, and the minimum detectable concentrations of iprobenfos in rice straw and husked rice samples were 2.0 and 0.5 μg/kg, respec- tively. [Conclusion] The established determination method is characterized by low de- termination limit, high sensitivity, good reproducibility and high operability, which all meet the requirements by Guideline on Pesticide Residue Trials of the Ministry of Agriculture.
基金support under the National Basic Research Program of China (2009CB421605)National Key Water Program(2009ZX07207-002-03)National Natural Science Foundation of China (20977096)
文摘Forty-eight vinegar samples including white vinegar, rice vinegar and mature vinegar were collected from several markets in Beijing. Butyltin compounds were determined by headspace solid-phase microextraction coupled with gas chromatography and flame photometric detector after in situ ethylation with sodium tetraethylborate. Butyltin species were detected in sixteen vinegar samples and ranged from 0.012 to 14.10 lag Sn L 1. The detection rate of white vinegar is higher than that of rice vinegar and mature vinegar. Vinegar samples with relatively high butyltin concentration (〉1.5 μg Sn L-1) were those stored in plastic bags, indicating that the plastic bag was one of the possible sources of butyltin contamination. This was further confirmed by the leaching experiments of three selected plastic bags, and monobutyltin was detected in the leaching solvents. According to the estimation, the average daily intake of total butyltin compounds through vinegar consumption is about 0.04 ng Sn/kg b.w., much lower than the Tolerable Daily Intake (TDI) of 100 ng Sn/kg b.w. set by the European Food Safety Authority (EFSA).
