ABSTRACT
OBJECTIVE: To establish a simple and sensitive method for simultaneous detection of chlorpyrifos( CPF),and its metabolite 3,5,6-trichloro-2-pyridinol( TCP) in plasma samples by ultra performance liquid chromatography( UPLC).METHODS: The 0. 5 m L of blood sample was extracted by ethyl acetate,then separated by C18 column using acetonitrile /water as a mobile phase and detected by diode-array detector under the ultraviolet spectrum of 298 nm( 0. 0-2. 0 min) and289 nm( 2. 0-5. 0 min) through UPLC. RESULTS: The method showed that a good linear range was 1. 00-50. 00 mg / L of both CPF and TCP,and the correlation coefficients was 0. 999 9. The limit of detection was 0. 30 mg / L and the lower limits of quantitation was 1. 00 mg / L of both CPF and TCP. The recovery rates of CPF and TCP were 87. 20 %-103. 08 %and 86. 20 %-99. 28 %,respectively. The within-run relative standard deviation( RSD) of CPF and TCP was 5. 28 %-6. 17 % and 2. 32 %-4. 43 %,and the between-run RSD was 6. 62 %-7. 53 % and 3. 55 %-5. 24 %. Samples can be kept in4 degrees Celsius refrigerator for 7 days. CONCLUSION:s The proposed method is simple,reliable and sensitive. It can be applied for simultaneous detection of CPF and its metabolite TCP in plasma samples.
ABSTRACT
OBJECTIVE: To establish a methodology for determining indium in human whole blood,serum and urine by inductively coupled plasma-mass spectrometry( ICP-MS). METHODS: The whole blood,serum and urine samples were diluted 10 times in 0. 01%( mass fraction) Triton X-100 plus 0. 50%( mass fraction) nitric acid solution,and the indium level was determined by ICP-MS. Rhodium standard solution was used as the internal standard control. RESULTS: The working curve obtained from measurement of whole blood,serum and urine of normal individuals was compared to the standard curve and showed no significant difference in quantitative analysis( P > 0. 05). The linearity range of indium concentration in whole blood,serum and urine was 0. 000-20. 000 μg / L,and all the correlation coefficients were greater than 0. 999 with a detection limit of 0. 144 μg / L. The recovery rates of whole blood,serum and urine were 87. 90%-95. 92%,91. 50%-94. 20% and 90. 40%-96. 57%,respectively. The relative standard deviations( RSDs) of within-run precision were 3. 81%-7. 05%,3. 75%-5. 90% and 4. 31%-6. 62%,respectively. The RSDs of between-run precision were 2. 90%-7. 10%,3. 80%-5. 92% and 4. 16%-5. 94%,respectively. Samples could be stored for at least 14 days under the temperature of- 20 ℃. The indium in whole blood,serum and urine of workers occupationally exposed to indium( exposure group,135 person-time) and control group workers( 120 person-time) were examined. Indium was detected for 17 person-time in whole blood and serum in the exposure group with a detection rate of 1. 26%. Indium was not detected in urine samples in exposure group. It was not detected in all samples in control group. CONCLUSION: This methodology has features of simple operation,high accuracy and good precision,which is suitable for the accurate quantitative analysis of indium in biological samples.
ABSTRACT
<p><b>OBJECTIVE</b>To establish a solvent desorption Gas chromatographic method for detecting the isoflurane in air of workplaces.</p><p><b>METHODS</b>This method is based on "Standardization of methods for determination of toxic substances in workplace air".</p><p><b>RESULTS</b>This method presents the linear relation with the minimum detectable limit 1.0 µg/ml and the minimum detectable concentration 0.07 mg/m(3). The precision (RSD) was 0.5% ∼ 5.0%, the mean dsorption efficiencies were 96.7% ∼ 98.9%, the absorption efficiencies were 92.1% ∼ 100%, the breakthrough volume was 3.7 mg isoflurane/100 mg active carbon. Other volatile organic solvents (Sevoflurane, Enflurane and Ethyl Alcohol) did not interfere the detection. The sample could be stored in the active carbon tube at least for 10 days.</p><p><b>CONCLUSION</b>This method is meet the requirement of GBZ/T 210.4-2008 "Guide for establishing occupational health standards-Part4: Determination methods of air chemicals in workplace" and is feasible for determining the isoflurane in the air of workplaces.</p>