To formulate a scientific basis for a reasonable spray dose and safe interval period of 20% flubendiamide water dispersible granule (WDG) on controlling vegetable pests, degradation dynamics of flubendiamide in cabbag...To formulate a scientific basis for a reasonable spray dose and safe interval period of 20% flubendiamide water dispersible granule (WDG) on controlling vegetable pests, degradation dynamics of flubendiamide in cabbage and soil was analyzed in this study. Dissipation and residue of flubendiamide in 20% flubendiamide WDG in cabbage and soil under field conditions were investigated by liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction. Results showed that the degradation dynamic equations of flubendiamide in cabbage and soil were based on the first-order reaction dynamic equations. The half-lives of the degradation of flubendiamide were 3.51 d to 3.96 d and 3.43 d to 3.87 d in the cabbage of Yangzhou and Jingzhou, respectively, and 4.42 d to 5.13 d and 4.37 d to 4.99 d in the soil of Yangzhou and Jingzhou, respectively. The terminal residues of flubendiamide in the cabbage of Yangzhou and Jingzhou were 0.0247 mg·kg-1 to 0.0393 mg·kg-1 and 0.0225 mg·kg-1 to 0.0273 mg·kg-1, respectively, when 20% flubendiamide WDG was applied at a dose of0.050g·m-2. Flubendiamide is safe to be applied in cabbage fields at the recommended dose.展开更多
A fast analytical method for the simultaneous determination of 9 mycotoxins, including alfatoxins （B1, B2, G1, and G2）, fumonisins （B1, B2 and B3）, zearalenone, and deoxynivalenol in corn using dispersive solid-ph...A fast analytical method for the simultaneous determination of 9 mycotoxins, including alfatoxins （B1, B2, G1, and G2）, fumonisins （B1, B2 and B3）, zearalenone, and deoxynivalenol in corn using dispersive solid-phase extraction method and ultra-performance liquid chromatography coupled to tandem quadrupole time-of-lfight mass spectrometry （UPLC-Q-TOF-MS） was developed and validated. Samples were extracted with acetonitrile-water （84：16, v：v, containing 1% acetic acid） using ultrasonic extraction. The extracts were puriifed with a dispersive SPE method using C18 as a cleaning agent. The ifnal clear extracts were dried by nitrogen blowing and subsequently redissolved in methanol-water （5：5, v：v）. The samples were then analyzed by UPLC-Q-TOF-MS with 0.1% formic acid in ammonium acetate-methanol as mobile phase. The mean recoveries were ranged from 68.0 to 120.0%, and the relative standard deviation （RSD） ranged from 0.18 to 6.29%. Limits of detections ranged from 0.05 to 50 μg kg？1, and limits of quantiifcation ranged from 0.1 to 200 μg kg？1, which were below the legal limits set by the European Union for the legislated mycotoxins. The developed method was applied to 130 corn samples. Among the mycotoxins studied, alfatoxins B1 and fumonisins B1, B2 and B3 were the most predominant mycotoxins, and their concentrations were 0–593.12, 0–2.01×104, 0–6.94×103 and 0–3.05×103 μg kg–1, respectively.展开更多
Matrix solid-phase dispersion（MSPD） was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determina...Matrix solid-phase dispersion（MSPD） was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determination of the analyte was carried out by high performance liquid chromatography with UV detection. The alkaline alumina was used as sorbent. The mixture of acetonitrile and water was used as elution solvent. Several extraction parameters, such as type of sorbent, the ratio of sample to solid support material, type of the elution solvent and the volume of the elution solvent were tested. Mean recoveries ranged from 93.16% to 102.73%, with relative standard deviations from 0.27% to 4.17%. With the extraction efficiency and time expenditure taken into account, MSPD extraction should be a comparatively good method.展开更多
In this work,Fe3O4-Al2O3@CNFs nanocomposite was synthesised and used as a nanosorbent in the ultrasound-assisted dispersive magnetic solid phase extraction(UA-DMSPE)of 17-beta estradiol(E2)in wastewater samples.The qu...In this work,Fe3O4-Al2O3@CNFs nanocomposite was synthesised and used as a nanosorbent in the ultrasound-assisted dispersive magnetic solid phase extraction(UA-DMSPE)of 17-beta estradiol(E2)in wastewater samples.The quantification of E2 was achieved using high performance liquid chromatography coupled with diode array detector(HPLC-DAD).Various parameters affecting the efficiency of this sample preparation technique were optimised to achieve excellent sensitivity and high recoveries of E2.Response surface methodology was utilised for optimisation of these parameters.Using the optimised conditions,the linear dynamic range was achieved in the range of 0.1e1000 mgL^-1and the correlation coefficient was found to be 0.9981.The preconcentration factor,enrichment factor,limit of detection(LOD)and limit of quantification(LOQ)were 67,169,0.025 mgL^-1and 0.083 mg L1,respectively.The relative standard deviation(%RSD)for the intraday(n?10)and interday(n?5 working days)were 1.8%and 3.3%,respectively.The developed UA-DMSPE/HPLC-DAD method was applied for the preconcentration and determination of E2 in wastewater samples.The obtained results indicated that E2 was present in the wastewater samples.展开更多
该研究建立了热水浴提取-分散固相萃取(DSPE)净化-超高效液相色谱-串联质谱(UPLC-MS/MS)测定枸杞干果、鲜果中氯酸盐和高氯酸盐含量的方法。试样用7 m L超纯水在60℃水浴中振荡提取30 min后,加入13 m L甲醇涡旋5 min,离心后上清液用C18...该研究建立了热水浴提取-分散固相萃取(DSPE)净化-超高效液相色谱-串联质谱(UPLC-MS/MS)测定枸杞干果、鲜果中氯酸盐和高氯酸盐含量的方法。试样用7 m L超纯水在60℃水浴中振荡提取30 min后,加入13 m L甲醇涡旋5 min,离心后上清液用C18和石墨化碳黑(GCB)组合分散固相萃取净化,净化液在电喷雾负离子源和多反应监测(MRM)模式下测定,基质外标法定量。结果表明,枸杞干果、鲜果中氯酸盐和高氯酸盐均分别在1.0~100.0 ng/mL、0.5~100.0 ng/mL范围内线性关系良好,相关系数R2分别为0.998 9和0.999 2及0.998 4和0.999 0。氯酸盐检出限(LOD)为1.0μg/kg、定量限(LOQ)为10.0μg/kg;高氯酸盐LOD为0.5μg/kg、LOQ为5.0μg/kg。干果中氯酸盐和高氯酸盐平均加标回收率分别为89.9%~93.4%和76.8%~93.6%,相对标准偏差(RSD)分别小于11.0%和12.0%;鲜果中氯酸盐和高氯酸盐平均加标回收率分别为73.8%~94.9%和61.2%~90.5%,RSD分别小于11.0%和17.0%。展开更多
文摘To formulate a scientific basis for a reasonable spray dose and safe interval period of 20% flubendiamide water dispersible granule (WDG) on controlling vegetable pests, degradation dynamics of flubendiamide in cabbage and soil was analyzed in this study. Dissipation and residue of flubendiamide in 20% flubendiamide WDG in cabbage and soil under field conditions were investigated by liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction. Results showed that the degradation dynamic equations of flubendiamide in cabbage and soil were based on the first-order reaction dynamic equations. The half-lives of the degradation of flubendiamide were 3.51 d to 3.96 d and 3.43 d to 3.87 d in the cabbage of Yangzhou and Jingzhou, respectively, and 4.42 d to 5.13 d and 4.37 d to 4.99 d in the soil of Yangzhou and Jingzhou, respectively. The terminal residues of flubendiamide in the cabbage of Yangzhou and Jingzhou were 0.0247 mg·kg-1 to 0.0393 mg·kg-1 and 0.0225 mg·kg-1 to 0.0273 mg·kg-1, respectively, when 20% flubendiamide WDG was applied at a dose of0.050g·m-2. Flubendiamide is safe to be applied in cabbage fields at the recommended dose.
基金supported by the Key Project of Science and Technology Development Program of Shandong Province,China(2013KF03)
文摘A fast analytical method for the simultaneous determination of 9 mycotoxins, including alfatoxins （B1, B2, G1, and G2）, fumonisins （B1, B2 and B3）, zearalenone, and deoxynivalenol in corn using dispersive solid-phase extraction method and ultra-performance liquid chromatography coupled to tandem quadrupole time-of-lfight mass spectrometry （UPLC-Q-TOF-MS） was developed and validated. Samples were extracted with acetonitrile-water （84：16, v：v, containing 1% acetic acid） using ultrasonic extraction. The extracts were puriifed with a dispersive SPE method using C18 as a cleaning agent. The ifnal clear extracts were dried by nitrogen blowing and subsequently redissolved in methanol-water （5：5, v：v）. The samples were then analyzed by UPLC-Q-TOF-MS with 0.1% formic acid in ammonium acetate-methanol as mobile phase. The mean recoveries were ranged from 68.0 to 120.0%, and the relative standard deviation （RSD） ranged from 0.18 to 6.29%. Limits of detections ranged from 0.05 to 50 μg kg？1, and limits of quantiifcation ranged from 0.1 to 200 μg kg？1, which were below the legal limits set by the European Union for the legislated mycotoxins. The developed method was applied to 130 corn samples. Among the mycotoxins studied, alfatoxins B1 and fumonisins B1, B2 and B3 were the most predominant mycotoxins, and their concentrations were 0–593.12, 0–2.01×104, 0–6.94×103 and 0–3.05×103 μg kg–1, respectively.
基金Supported by the Projects in the National Science & Technology Pillar Program During the Eleventh Five-Year Plan Period of China(No 2006BAI14B01)
文摘Matrix solid-phase dispersion（MSPD） was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determination of the analyte was carried out by high performance liquid chromatography with UV detection. The alkaline alumina was used as sorbent. The mixture of acetonitrile and water was used as elution solvent. Several extraction parameters, such as type of sorbent, the ratio of sample to solid support material, type of the elution solvent and the volume of the elution solvent were tested. Mean recoveries ranged from 93.16% to 102.73%, with relative standard deviations from 0.27% to 4.17%. With the extraction efficiency and time expenditure taken into account, MSPD extraction should be a comparatively good method.
基金the Department of Science and Technology(DST,South Africa)/National Nanoscience Postgraduate Teaching and Training Programme(NNPTTP)and National Research Foundation(NRF,South Africa,grant no.99270&91230).
文摘In this work,Fe3O4-Al2O3@CNFs nanocomposite was synthesised and used as a nanosorbent in the ultrasound-assisted dispersive magnetic solid phase extraction(UA-DMSPE)of 17-beta estradiol(E2)in wastewater samples.The quantification of E2 was achieved using high performance liquid chromatography coupled with diode array detector(HPLC-DAD).Various parameters affecting the efficiency of this sample preparation technique were optimised to achieve excellent sensitivity and high recoveries of E2.Response surface methodology was utilised for optimisation of these parameters.Using the optimised conditions,the linear dynamic range was achieved in the range of 0.1e1000 mgL^-1and the correlation coefficient was found to be 0.9981.The preconcentration factor,enrichment factor,limit of detection(LOD)and limit of quantification(LOQ)were 67,169,0.025 mgL^-1and 0.083 mg L1,respectively.The relative standard deviation(%RSD)for the intraday(n?10)and interday(n?5 working days)were 1.8%and 3.3%,respectively.The developed UA-DMSPE/HPLC-DAD method was applied for the preconcentration and determination of E2 in wastewater samples.The obtained results indicated that E2 was present in the wastewater samples.
