A novel method for determination of formaldehyde sulfoxylate,sulfite,thiocyanate,and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed.All specie...A novel method for determination of formaldehyde sulfoxylate,sulfite,thiocyanate,and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed.All species are separated at Dionex IonPac AG22A and AS22A with mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0mL/min.The postcolumn derivation solution was 0.24%iodine in 0.2%phosphate acid and the detection wavelength was set at 288 nm.The detection limits(LOD,signal-to-noise ratio of 3) of formaldehyde sulfoxylate,sulfite, thiocyanate,and thiosulfate were 0.004,0.006,0.006,and 0.007 mg/L,respectively.Within-day relative standard deviations(RSD, n = 10) of formaldehyde sulfoxylate,sulfite,thiocyanate,and thiosulfate were 3.24%,3.76%,2.68%,and 2.07%,respectively.The recoveries of the four anions were in the range of 67.2-116.5%.展开更多
A method has been developed for separation of 20 kinds of aromatic carboxylic acid using anion-exchange chromatography. A Dionex IonPac AS9-HC guard column (250mm×2mm) was used with a 9mmol/L sodium carbonate sol...A method has been developed for separation of 20 kinds of aromatic carboxylic acid using anion-exchange chromatography. A Dionex IonPac AS9-HC guard column (250mm×2mm) was used with a 9mmol/L sodium carbonate solution containing 50% (v/v) acetonitrile as eluent. A set of retention time data has been obtained using a conductivity detector DS6. Furthermore, geometrical optimization and electrostatic potential calculation of 20 kinds of aromatic carboxylic acid have been performed at the HF/6-31G* level of theory. A number of statistically-based parameters derived from molecular surface electrostatic potential have been obtained. Linear relationship between retention time and structural parameters has been established by multiple regression method. The result shows that parameters derived from electrostatic potential Vs +, Vs -, П together with the dipole moment μ can be well used to express the quantitative structure-retention time of this kind of aromatic carboxylic acid. Good predictive capability has also been demonstrated. The result has provided a framework which further proves the general applicability of this electrostatic potential parameter set to a great extent,and with which the ion chromatographic adsorption mechanism can be investigated.展开更多
This paper presents a novel method for simultaneous online examination of free aluminum ions(Al3+)in seafood,using solidphase extraction and high-performance liquid chromatography online with inductively coupled plasm...This paper presents a novel method for simultaneous online examination of free aluminum ions(Al3+)in seafood,using solidphase extraction and high-performance liquid chromatography online with inductively coupled plasma mass spectrometry(SPEHPLC-ICP-MS),without post-column reaction.The optimum conditions for chromatographic separation of Al3+were achieved using an IonPac CS5A analytical column with an IonPac CG5A guard column.The mobile phase consisted of 0.040 mol/L LiOH,0.0060 mol/L 2,6-pyridinedicarboxylic acid,and 0.090 mol/L CH3COOH(pH 4.7).The free Al3+ions in seafood were extracted by shaking with the mobile phase at 70°C for 2 h.SPE was conducted using an Oasis MCX,3cc/60 mg,30μm column,which was activated and equilibrated with 2 mL of methanol and 4 mL of deionized water before use.HCl(0.075 mol/L,2 mL)was used to wash inorganic Al from the SPE column.The standard recoveries of Al3+were all above 89%and the relative standard deviations were all below 5%.The proposed method was successfully used for the examination of Al3+in seafood samples,and the results were similar to those obtained using the static equilibrium method.展开更多
A new method was developed for simultaneous determination of levels of AMP,ADP and ATP in blood by anion-exchange chromatography.The three adenosine phosphates were separated by Dionex IonPac AG18(50 mm×4 mm) gua...A new method was developed for simultaneous determination of levels of AMP,ADP and ATP in blood by anion-exchange chromatography.The three adenosine phosphates were separated by Dionex IonPac AG18(50 mm×4 mm) guard column and IonPac AS 18(250 mm×4 mm) analytical column using a gradient method and detected with a suppressed conductivity detector. The detection limits(S/N=3) of AMP,ADP and ATP were 38,47,108 ng/L,respectively.The relative standard deviations of retention time,peak area and peak height were all less than 1.87%and a good linear relationship was obtained.This method was applied to analyze human blood samples.展开更多
基金supported by National Natural Science Foundation of China(No.20775070) Zhejiang Provincial Natural Science Foundation of China(No.Y507252)+1 种基金Zhejiang Qianjiang Project of Science and Technology for Competent People(No.2008R10028) Zhejiang Provincial Analysis and Testing Foundation of China(No.2007F70061)
文摘A novel method for determination of formaldehyde sulfoxylate,sulfite,thiocyanate,and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed.All species are separated at Dionex IonPac AG22A and AS22A with mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0mL/min.The postcolumn derivation solution was 0.24%iodine in 0.2%phosphate acid and the detection wavelength was set at 288 nm.The detection limits(LOD,signal-to-noise ratio of 3) of formaldehyde sulfoxylate,sulfite, thiocyanate,and thiosulfate were 0.004,0.006,0.006,and 0.007 mg/L,respectively.Within-day relative standard deviations(RSD, n = 10) of formaldehyde sulfoxylate,sulfite,thiocyanate,and thiosulfate were 3.24%,3.76%,2.68%,and 2.07%,respectively.The recoveries of the four anions were in the range of 67.2-116.5%.
基金Supported by the Project of Analysis and Detection of Zhejiang Province in 2009 (No. 2009F7044)
文摘A method has been developed for separation of 20 kinds of aromatic carboxylic acid using anion-exchange chromatography. A Dionex IonPac AS9-HC guard column (250mm×2mm) was used with a 9mmol/L sodium carbonate solution containing 50% (v/v) acetonitrile as eluent. A set of retention time data has been obtained using a conductivity detector DS6. Furthermore, geometrical optimization and electrostatic potential calculation of 20 kinds of aromatic carboxylic acid have been performed at the HF/6-31G* level of theory. A number of statistically-based parameters derived from molecular surface electrostatic potential have been obtained. Linear relationship between retention time and structural parameters has been established by multiple regression method. The result shows that parameters derived from electrostatic potential Vs +, Vs -, П together with the dipole moment μ can be well used to express the quantitative structure-retention time of this kind of aromatic carboxylic acid. Good predictive capability has also been demonstrated. The result has provided a framework which further proves the general applicability of this electrostatic potential parameter set to a great extent,and with which the ion chromatographic adsorption mechanism can be investigated.
基金supported by the Agricultural Industry Standard of thePeople’s Republic of China(2011516)the National Natural Science Foundation of China(41206101)+1 种基金the Special Fund of Chinese General Government for Basic Scientific Research Operations in Commonweal Research Institutes(20603022012016)National Key Technology R&D Program of the Ministry of Science and Technology(2011BAD13B06)
文摘This paper presents a novel method for simultaneous online examination of free aluminum ions(Al3+)in seafood,using solidphase extraction and high-performance liquid chromatography online with inductively coupled plasma mass spectrometry(SPEHPLC-ICP-MS),without post-column reaction.The optimum conditions for chromatographic separation of Al3+were achieved using an IonPac CS5A analytical column with an IonPac CG5A guard column.The mobile phase consisted of 0.040 mol/L LiOH,0.0060 mol/L 2,6-pyridinedicarboxylic acid,and 0.090 mol/L CH3COOH(pH 4.7).The free Al3+ions in seafood were extracted by shaking with the mobile phase at 70°C for 2 h.SPE was conducted using an Oasis MCX,3cc/60 mg,30μm column,which was activated and equilibrated with 2 mL of methanol and 4 mL of deionized water before use.HCl(0.075 mol/L,2 mL)was used to wash inorganic Al from the SPE column.The standard recoveries of Al3+were all above 89%and the relative standard deviations were all below 5%.The proposed method was successfully used for the examination of Al3+in seafood samples,and the results were similar to those obtained using the static equilibrium method.
基金financially supported by National Natural Science Foundation of China(Nos.20775070 and J0830413)Zhejiang Provincial Natural Science Foundation of China(Nos.R4080124 and Y4090268)
文摘A new method was developed for simultaneous determination of levels of AMP,ADP and ATP in blood by anion-exchange chromatography.The three adenosine phosphates were separated by Dionex IonPac AG18(50 mm×4 mm) guard column and IonPac AS 18(250 mm×4 mm) analytical column using a gradient method and detected with a suppressed conductivity detector. The detection limits(S/N=3) of AMP,ADP and ATP were 38,47,108 ng/L,respectively.The relative standard deviations of retention time,peak area and peak height were all less than 1.87%and a good linear relationship was obtained.This method was applied to analyze human blood samples.