An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracte...An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics.展开更多
A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 s...A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.展开更多
To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry ...To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.展开更多
A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established....A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established. Firstly,environmental water samples were extracted by disk SPE column( C_(18)),and three kinds of MCs were separated by Waters BEH C_(18) chromatographic column with acetonitrile- 0. 2% formic acid solution as the mobile phase. After the gradient elution separation,the external standard method was used for quantitative and qualitative analysis under MRM of UPLC- MS / MS. The results showed that the three kinds of MCs in the range of 0. 05- 10 μg / L showed good linear relation,and the correlation coefficients were higher than 0. 999 4,while the method detection limit was 0. 04 ng / L. Under 0. 1,1,and 5 μg / L standard addition for the same environmental sample,the average recovery was 82. 8%- 108. 8%,and the relative standard deviation of determination results was2. 1%- 10. 1%( n = 6). This method is rapid,sensitive and accurate,so it can be effectively applied in the monitoring of MCs in environmental water samples.展开更多
[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an H...[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an HLB solid-phase extraction column was activated, and a water sample, which was adjusted with phosphoric acid to a pH of (2±0.5) and added with 500 mg of disodium EDTA, was loaded, and 5 ml of water and 20% methanol water was added for washing. Next, 10 ml of elution solution was added for elution, and the collected eluate was evaporated under reduced pressure at 40 ℃ to near dryness, and 1 ml of reconstitution solution was added to a constant volume. An ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 2.6 μm) chromatographic column was adopted for LC separation by gradient elution with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase. For MS detection, the MRM mode was adopted for collection, and the positive and negative ion modes were switched for simultaneous determination, and the internal standard method was used for quantification. [Results] The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance. The limits of detection ranged from 0.15 to 3.00 ng/L, and the limits of quantitation were between 0.80 and 10.00 ng/L, and the recoveries ranged from 77.9% to 104.85%. [Conclusions] The method has high sensitivity, good accuracy and strong practical value.展开更多
The method of simultaneous analysis of Sudan Red Ⅰ-Ⅳ residues in ketchup was developed with an ultra performance liquid chromatography-tandem mass spectrum.Acetonitrile was used to extract the substance from the ket...The method of simultaneous analysis of Sudan Red Ⅰ-Ⅳ residues in ketchup was developed with an ultra performance liquid chromatography-tandem mass spectrum.Acetonitrile was used to extract the substance from the ketchup,and the upper layer was detected by the UPLC-MS/MS after refrigeration and centrifuge.The sample was separated on a Waters Acquity BHE C18 column,and detected by the MRM mode of the mass spectrum.The LOD was 2 ng/mL and the LOQ was 5 ng/mL all of the four substances.The average recoveries were between 67.42%-84.59% of the 100,200,300 μg/kg three spiked concentration levels and the RSD values were between 2.87%-9.57%.展开更多
An ultra performance liquid chromatography-tandem mass spectrum method has been developed for the determination of three aconitum alkaloids (aconitine,hypaconitine and mesaconitine).The three alkaloids were analyzed s...An ultra performance liquid chromatography-tandem mass spectrum method has been developed for the determination of three aconitum alkaloids (aconitine,hypaconitine and mesaconitine).The three alkaloids were analyzed simultaneously with an Waters Acquity BHE C18 column by gradient elution using 0.05% aqueous ammonia-acetonitrile as mobile phase and detected by the MRM mode of the mass spectrum.The recoveries of the SPE method were between 68.79%-95.65% (RSD<7.94%,n=4),and all the alkaloids showed good linearity (r>0.998) in a relatively wide concentration range.The LOD reached 0.0516,0.0640,0.0744 ng/mL of aconitine,hypaconitine and mesaconitine,respectively.The analysis time was within 3 min which could meet the high-throughput detection.The results indicated that contents of alkaloids in animal blood can be well detected;and this method can be used in quality control of aconitum drugs and pharmacokinetics study.展开更多
文摘An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics.
基金supported by the Natural Science Foundation of Zhejiang Province,China(No.LY17C200009)the Foundation of Zhejiang Educational Committee(No.Y201328477)
文摘A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
文摘A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established. Firstly,environmental water samples were extracted by disk SPE column( C_(18)),and three kinds of MCs were separated by Waters BEH C_(18) chromatographic column with acetonitrile- 0. 2% formic acid solution as the mobile phase. After the gradient elution separation,the external standard method was used for quantitative and qualitative analysis under MRM of UPLC- MS / MS. The results showed that the three kinds of MCs in the range of 0. 05- 10 μg / L showed good linear relation,and the correlation coefficients were higher than 0. 999 4,while the method detection limit was 0. 04 ng / L. Under 0. 1,1,and 5 μg / L standard addition for the same environmental sample,the average recovery was 82. 8%- 108. 8%,and the relative standard deviation of determination results was2. 1%- 10. 1%( n = 6). This method is rapid,sensitive and accurate,so it can be effectively applied in the monitoring of MCs in environmental water samples.
基金Supported by Tongren Science and Technology Planning Project(TSKY[2022]42)Science Planning Project of Department of Education of Guizhou Province(2023B111)。
文摘[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an HLB solid-phase extraction column was activated, and a water sample, which was adjusted with phosphoric acid to a pH of (2±0.5) and added with 500 mg of disodium EDTA, was loaded, and 5 ml of water and 20% methanol water was added for washing. Next, 10 ml of elution solution was added for elution, and the collected eluate was evaporated under reduced pressure at 40 ℃ to near dryness, and 1 ml of reconstitution solution was added to a constant volume. An ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 2.6 μm) chromatographic column was adopted for LC separation by gradient elution with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase. For MS detection, the MRM mode was adopted for collection, and the positive and negative ion modes were switched for simultaneous determination, and the internal standard method was used for quantification. [Results] The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance. The limits of detection ranged from 0.15 to 3.00 ng/L, and the limits of quantitation were between 0.80 and 10.00 ng/L, and the recoveries ranged from 77.9% to 104.85%. [Conclusions] The method has high sensitivity, good accuracy and strong practical value.
文摘The method of simultaneous analysis of Sudan Red Ⅰ-Ⅳ residues in ketchup was developed with an ultra performance liquid chromatography-tandem mass spectrum.Acetonitrile was used to extract the substance from the ketchup,and the upper layer was detected by the UPLC-MS/MS after refrigeration and centrifuge.The sample was separated on a Waters Acquity BHE C18 column,and detected by the MRM mode of the mass spectrum.The LOD was 2 ng/mL and the LOQ was 5 ng/mL all of the four substances.The average recoveries were between 67.42%-84.59% of the 100,200,300 μg/kg three spiked concentration levels and the RSD values were between 2.87%-9.57%.
文摘An ultra performance liquid chromatography-tandem mass spectrum method has been developed for the determination of three aconitum alkaloids (aconitine,hypaconitine and mesaconitine).The three alkaloids were analyzed simultaneously with an Waters Acquity BHE C18 column by gradient elution using 0.05% aqueous ammonia-acetonitrile as mobile phase and detected by the MRM mode of the mass spectrum.The recoveries of the SPE method were between 68.79%-95.65% (RSD<7.94%,n=4),and all the alkaloids showed good linearity (r>0.998) in a relatively wide concentration range.The LOD reached 0.0516,0.0640,0.0744 ng/mL of aconitine,hypaconitine and mesaconitine,respectively.The analysis time was within 3 min which could meet the high-throughput detection.The results indicated that contents of alkaloids in animal blood can be well detected;and this method can be used in quality control of aconitum drugs and pharmacokinetics study.