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{L-End}Objective To establish a method for the simultaneous determination of dimethyltin (DMT), trimethyltin (TMT), diethyltin (DET), and triethyltin (TET) in human whole blood using high performance liquid chromatography-inductively coupled plasma-mass spectrometry (ICP-MS). {L-End}Methods The 1.0 mL of blood was added with 4.0 mL 65% aqueous solution (containing 6% acetic acid), extracted and separated by C4 column (150 mm×3 mm×3 μm) using a mobile phase of methanol and 4% acetic acid aqueous solution (containing 0.25 mmol/L tropolone) at a volume ratio of 35∶65, and detected by ICP-MS. {L-End}Results The linear range of DMT, TMT, DET, and TET was 30.60-550.80, 29.00-522.00, 46.10-829.80, and 34.05-612.90 μg/L, respectively. All correlation coefficients were 0.999. The detection limit of DMT, TMT, DET and TET was 21.40, 20.30, 32.27 and 23.80 μg/L, respectively. The recovery rate was 81.9%-104.9%. The within-run and between-run relative standard deviation was 1.6%-6.9% and 0.1%-10.0%, respectively. The samples can be stored at -20 ℃ and 4 ℃ for at least three days. {L-End}Conclusion This method can be used for trace analysis of DMT, TMT, DET, and TET in whole blood.
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OBJECTIVE: To establish a detecting method for sulfur dioxide in workplace air by molecular sieve solid adsorption tube sampling and ion chromatography. METHODS: Air samples were collected by molecular sieve solid adsorption tubes,desorbed by distilled water,oxidized by hydrogen peroxide in weak base system,separated by anion exchange chromatography and detected by conductivity detector. RESULTS: The good linearity range of sulfur dioxide was0. 10-16. 00 mg/L,and the correlation coefficient was 0. 999 8. The detection limit was 0. 02 mg/L,the minimum detectable concentration was 0. 01 mg/m3. The average desorption efficiency was 96. 53%-99. 35%. The within-run and between-run relative standard deviations were 1. 73%-3. 65% and 1. 80%-4. 46% respectively. The samples could be stored at room temperature for at least 14 days. CONCLUSION: This method is suitable for detecting sulfur dioxide in workplace air.
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OBJECTIVE: To establish a method for detecting human urinary thiocyanate by gas chromatographic and pre-column derivatization with 2,3,4,5,6-pentafluorobenzyl bromide( PFB-Br). METHODS: A total of 20. 0 μL of urine was taken and 1. 0 m L of acetonitrile and 100. 0 μL of PFB-Br were added for derivative reaction. The gas chromatography was directly used for measurement. RESULTS: The urinary thiocyanate concentration showed a good linear range of 1. 000-10. 000 mg/L. The linear correlation coefficient was 0. 999 6. The minimum detection concentration was 0. 112 mg/L,and the minimum quantitative concentration was 0. 411 mg/L( 20. 0 μL urine sample). The standard recovery rate was 97. 22%-102. 04%.The within-run relative standard deviation( RSD) of this method was 1. 56%-5. 35%. The between-run RSD was 1. 46%-5. 10%. Hydrocyanic acid ions interfered with the measurement. Other common inorganic ions such as chloride,sulfate,and nitrate ions did not interfere with the measurement results. The samples can be stored at 4 ℃ for at least 15 days. CONCLUSION: This method is suitable for detecting human urinary thiocyanate.
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OBJECTIVE: To explore the feasibility of simultaneous detection of 45 kinds of common organic compounds in workplace air by solvent desorption-gas chromatography method.METHODS: A total of 45 kinds of common organic compounds such as benzene,1,2-dichloroeyhane,n-hexane and trichloroethylene in workplace air were collected with activated carbon tube and desorbed with carbon disulfide,separated by capillary chromatographic column,and detected with flame ionization detector.RESULTS: There was good linear relationship in the selected range.The correlation coefficients was 0.999 92-0.999 99.The detection limit was 0.03-0.30 mg/L and the minimum detectable concentration range was 0.01-0.20 mg/m~3( sample volume was 3.00 L).The average desorption efficiencies was 75.4%-105.7%.The within-run and between-run relative standard deviations were 0.4%-6.7% and 1.8%-7.9%,respectively.The sampling efficiency was 91.9%-100.0%.CONCLUSION: The method is simple,high sensitivity and good precision,which can be used for simultaneous detection of 45 kinds of common coexisting organic compounds in workplace air.
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OBJECTIVE: To establish a method for detecting thiocyanate in human urine by high performance liquid chromatography( HPLC) with 2,3,4,5,6-pentafluorobenzyl bromide as precolumn derivatization reagent.METHODS: Thiocyanate in human urine was derived with 2,3,4,5,6-pentafluorobenzyl bromide, and separated by poroshell 120EC-C18 column with acetonitrile:deionized water( 60:40,V/V) as mobile phase.detected by HPLC,Liquid chromatography-UV detector was used for determination.The wavelength was 212.00 nm.RESULTS: Good linearity was obtained in the range of 0.05-10.32 mg/L with the correlation coefficient of 0.999.The detection limit was 6.31 μg/L and the minimum detection concentration was 63.10 μg/L( 0.1 mL urine).The recovery rate was 95.1%-102.9%.The within-run relative standard deviation( RSD) and the between-run RSD were 0.9%-1.0% and 0.9%-2.1%,respectively.The urine samples could be stored at 4 ℃ for 7 days.CONCLUSION: This method has high sensitivity,good specificity and sample preparation,which can be used for detecting urine thiocyanate in occupational population.
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OBJECTIVE: To establish a method for detecting hexamethylene diamine in workplace air by high performance liquid chromatography( HPLC).METHODS: Hexamethylene diamine in the workplace air was collected by silica gel tube,and each was added with a concentration of 0.05 mol/L sodium bicarbonate solution,each with 0.60 mL of dansyl chloride solution( a mass concentration of 240.00 mg/L),and the volume was adjusted to 5.00 mL with acetonitrile,heating for 40.00 min in bath water,acetonitrile:water( 75:25,V/V) as the mobile phase,quantitated by the standard curve method,using HPLC for determinationstandard.RESULTS: The linear range of hexamethylene diamine was 0.040 0-6.000 0 mg/L,the correlation coefficient was 0.999 3,and the detection limit was 0.003 8 mg/L,and the minimum detection concentration was 0.002 5 mg/m~3( calculated by sample volume of 3.0 L); The within-run relative standard deviation( RSD) was 2.1%-3.0%,and the between-run RSD was 2.9%-3.6%.The average desorption efficiency of the method was 91.4%-94.1%.The sampling efficiency was 98.5%-99.6%.CONCLUSION: The method is simple,rapid,sensitive,accurate and suitable for the detecting hexamethylene diamine concentration in workplace air.
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Objective@#Study the response of GMDTC to cadmium ions and metal ions in vivo to determine whether GMDTC are specifically complexed with cadmium ions to provide a reference for the safety and dfficacy of GMDTC.@*Methods@#Complexometric titration, HPLC and HPLC-MS were applied to research the complexation reaction of GMDTC and various metal ions. The molecular ion peak of GMDTC, GMDTC-Cd complex and GMDTC-Pb complex also detected by LC-MS. Additionally, the initial structure was determined by DFT simulation method.@*Results@#Results of complexometric titration and HPLC detection showed that GMDTC characteristic absorption peak area was proportional to the concentration of itself and there was no color change and peak time change when the GMDTC mixed with Ca2+, Fe2+, Mg2+, Zn2+. However, the color changed to black transition when the GMDTC mixed with Cu2+ and the color changed from yellow precipitate to light yellow transparent transition when GMDTC mix with Hg2+. Moreover, the peak area as well as the retention time has changed a lot which indicated that a chemical reaction has already happened. When the GMDTC mixed with Cd2+ and Pb2+, the color has changed from pale yellow to colorless transparent and the peak area of GMDTC has increased a lot. Finally, the GMDTC-Cd complex ratio both of which are 2:1 were calculated based on the results of LC-MS instrument and atomic calculations.@*Conclusion@#The specific cadmium chelating agent GMDTC can not react with the Ca2+, Fe2+, Mg2+, Zn2+, but it can react chemically with Cu2+ and Hg2+, even specific complex with Pb2+ and Cd2+.
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OBJECTIVE: To establish a methodology for simultaneous detection of chloromethyl methyl ether( CMME) and bis-chloromethyl ether( BCME) in workplace air by gas chromatography. METHODS: CMME and BCME in workplace air were collected with absorption solution which was also derivatization solution. The derivative products were extracted using n-hexane alkaline medium. The extracts were separated by capillary column and detected with electron capture detector.The quantification was performed by use of standard curves. RESULTS: The linearity ranges of CMME and BCME were2. 00-80. 00 and 1. 32-52. 80 ng,respectively. The correlation coefficients were both 0. 999 93. The minimum detectable concentrations were both 0. 030 μg / m3 and the minimum quantification concentrations were both 0. 100 μg / m3( 7. 50 L sample). The recovery rates were 99. 35%-101. 00% and 97. 99%-101. 70% respectively. The within-run relative standard deviations( RSD) were 2. 73%-4. 46% and 2. 61%-3. 82% respectively,and the between-run RSD were3. 10%-5. 50% and 3. 89%-5. 38% respectively. The sampling efficiencies were 92. 43%-96. 25% and 91. 43%-94. 03%respectively. The samples were stable at room temperature for at least 15 days. CONCLUSION: This method is suitable for simultaneous detection of CMME and BCME in workplace air.
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Objective@#To develop a new solid sorbent tube for capturing glycidyl methacrylate (GMA) in workplace air, and establish a complete set of method.@*Methods@#GMA in workplace air was captured by the new solid sorbent tube filled with carbon aerogel adsorbent, desorbed with solution of 50% (V/V) dimethylformamide-carbon disulfide, separated through capillary chromatographic column, and then analyzed by gas chromatography-flame ionization detector.@*Results@#The linear range of GMA was 0.38-604.80 mg/L, and the related coefficient was 0.999 82. The within-run and the between-run precision were 1.11%-2.80% and 2.53%-4.84% respectively. The average desorption efficiency was 93.20%-94.97%. The minimum quantification concentration and The minimum quantification concentration were 0.02 and 0.07 mg/m3 respectively (3.00 L sample) . Samples could be stored for at least 8 days at room temperature.@*Conclusion@#The newly developed solid sorbent tube and its complete set of gas chromatography method is simple, and has high sensitivity and precision, so it can be used for sampling and quantitative detection of GMA in workplace air.