RESUMO
【Objective】 To establish gas chromatography for the determination of tributyl phosphate(TBP) residues in human prothrombin complex and then verify it. 【Methods】 Acid modified polyethylene glycol(PEG)(20M) capillary column was used with n-hexane as solvent. The chromatographic parameters were as follows: gasification chamber temperature at 220 ℃, column temperature at 155 ℃, detector temperature at 220 ℃, column flow rate at 2.0 mL/min, carrier gas as N2, detector as FID, and collection time for 10min. The accuracy, repeatability, linearity, specificity, intermediate precision, detection limit, quantitative limit, range and durability were verified. 【Results】 The verification results showed that the method had good specificity. The linear regression correlation coefficient of standard curve was 0.999 90. The recovery rate were 98.4%, 97.5% and 95.7% when the concentration at 50%, 100%(30μg/mL) and 150%, respectively, with an average recovery of 97.2% and a relative deviation of 2.15%. When the concentration was 100%, the repeatability was 2.08%, and the relative deviation of intermediate precision was 1.63%. The detection limit was 0.255 μg/mL, and the quantitative limit was 0.511 μg/mL. After changing capillary chromatographic columns with different batch numbers but the same types and manufacturer, the applicability test of the system met the requirements, and the method had good durability. 【Conclusion】 This method can be used for the determination of TBP residues of human prothrombin complex in laboratory.
RESUMO
Objective@#To put forward the suggestion of the occupational contact limit of tributyl phosphate in the air of the workplace.@*Methods@#Data of production and usage, workers' basic information, occupational history, and physical examinations were collected, and the environmental and individual levels of exposure were monitored using fixed-point and individual sampling. The results of the questionnaire and health examination were statistically analyzed using exact probability method of Fisher in the workers exposed to tributyl phosphate and the control group.@*Results@#The results showed that tributyl phosphate was widely distributed in the workplace of production and using enterprises, and the concentration of tributyl phosphate in packaging area was highest at 2.47 mg/m3, and in feeder nose was highest at 2.13 mg/m3. The discomfort symptoms were classified and results showed that tributyl phosphate exposure group of 136 people, all symptoms of 128 people, accounting for 94.44% of the total, the remaining 5.56% of the staff report had psychiatric symptoms or lethargy and irritability skin itching, the control group had no symptoms. There is or not discomfort symptoms in the tributyl phosphate exposure group and the control group was compared with the exact probability of Fisher, and the difference was statistically significant (P<0.05) . The results of healthy physical examination of workers exposed to tributyl phosphate and control group were statistically analyzed by the exact probability method of Fisher. The results showed that there was no significant difference in the results of routine internal medical examination, nervous system examination, skin examination, five senses examination, blood routine, urine routine, lung ventilation, and X ray chest fluoroscopy between the tributyl phosphate exposure group and the control group (P<0.05) .@*Conclusion@#The workplace permissible time-weighted tributyl phosphate and short-term exposure limit concentrations in China were set at 2.5 mg/m3 and 5 mg/m3, respectively.
RESUMO
Objective@#To establish a practical method forsampling and detectingtributyl phosphate intheworkplace.@*Methods@#The samples were extracted by glass fiber membrane, eluted with ether, separated by gas chromatography, and detected by flame photometric detector.@*Results@#There were good linear relationship in the minimum detection concentration was 7.2-720.0 μg/ml, and the correlation coefficient was 0.999 92. The detection limit was 0.86 μg/ml, and the minimum detection concentration was 0.14 mg/m3 (sample volume was 30 L) . Recovery rates were 99.8%-100.2%. The with-in relative standard deviations were 4.0%-5.4% and the between relative standard deviations were 2.0%-5.5%, and average samplingefficiency was about 99.1%-100.0%.@*Conclusion@#This method conforms with the requirements of "Standardization of Methods for Determination of Toxic Substance in Workplace" . Tributyl phosphate in air could be determined accurately using this method.