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Objective@#To development of ethylene glycol samples in silicone tubes, and the samples were applied to inter-laboratory comparison, through it to evaluate the detection capacity of occupational health testing laboratories.@*Methods@#Three content levels of ethylene glycol samples in silicone tubes were prepared, and the homogeneity and stability of samples were investigated, the results were statistically analyzed. A robust statistical four-point distance method was used to calculate the results submitted by each participant laboratory and the test capability of the laboratory was assessed by the z-score method.@*Results@#The statistic of the homogeneity of ethylene glycol samples in silicone tubes were less than the critical value (P>0.05) , and the samples were stable at room temperature for one month. The satisfactory rate of comparison between 204 laboratories was 88.24%.@*Conclusion@#The homogeneity and stability of the ethylene glycol samples in the silicone tubes can meet the requirements of proficiency testing and can be used for laboratory comparison. Most of the laboratories that participated in the comparison had the ability to detect ethylene glycol.
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Objective@#To develop a method for determination of metabolites of diphenylmethane diisocyanate (MDI) in urine, i.e. methylenedianiline (MDA) by high performance liquid chromatography-tandem mass (LC-MS-MS) . @*Methods@#Urine samples were prepared by hydrolyzation with sulfuric acid and extraction by acetonitrile, and then separated on a Shim-pack XR-ODS column, analyzed with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) . The external solvent standard calibration were tested. @*Results@#The linearity ranges were 0.05~20.00 μg/L, The related coefficients were 0.999 5. The limit of detection was 0.02 μg/L. The rats of recovery were 91.0%~103.4%. The relative standard deviations were between 2.7%~7.3%. @*Conclusion@#The method was sensitive, accurate and suitable for the MDA determination in urine of MDI exposed population.
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Objective@#To revise the standard method for the determination of phenylglyoxylic acid(PGA)and mandelic acid(MA) in urine by ultra-performance liquid chromatography.@*Methods@#The original standard method was evaluated by experiment, and the chromatographic column, the detection limit,quantitation limit and stabilityof the method were studied.@*Results@#The samples were separated by BEH Phenyl(50mm×2.1mm×1.7μm)column and the internal standard working curve method was used. The regression equations were y=3.660 7x+0.066 3 and y=5.161 2x-0.007 3 for MA and PGA respectively. Linear correlation coefficients were 0.999 3 and 0.999 1. Linearity ranges were 0.10-1.00 mg/ml,0.04-0.40 mg/ml. The recoveries of PGA and MA were 91.6%-97.1% and 84.3%-99.0%,the precision were 0.9%-4.6% and 0.5%-1.9%. The detection limit and quantitation limit of the method were 1.1 mg/L and 3.7 mg/L for PGA, 5.4 mg/L and 17.9 mg/L for MA.@*Conclusion@#The method uses the phenyh modified chromatographic column, determines the detection limit. The method can improve quantitation limit, the detection accuracy and meet the detection of occupational population samples.
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Objective@#To establish the method for determination of titanium dioxide in the air of workplace by inductivehy coupled plasma optical emission spectrometry (ICP-OES) .@*Methods@#The titanium dioxide was collected by filter membrane and then digested by microwave digestion apparatus in the mixed solvents (HNO3∶HF∶H2O=4∶1∶1) , dilutedto 25 ml and detected by ICP-OES.@*Results@#The sampling efficiency was higher than 95%; the linearity of ICP-OES was good at the range of 10-500 μg/ml, the minimum quantitation concentration was 0.72 mg/m3 (as collecting 150 L air sample) , the maximum quantitation concentration was 21.7 mg/m3 (as collecting 960 L air sample) , the recovery was ranged from 99.0%-102.0%, the RSD of intra- and inter-batch precision were 0.5%-3.2% and 1.7%-3.5%, respectively.@*Conclusion@#The sampling method and determination method meet the requirements of guide for establishing occupational health standards-part 4: determinatin methods of air chemicals in workplace (GBZ/T 210.4-2008) , and areapplys to the collection and determination of TiO2 in the air of workplace.
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Objective@#To establish the method for determination of iron and its inorganic oxide in the air of workplace.@*Methods@#The iron and its inorganic oxide was collected by MCE filter membrane and then digested by electric heating digestion apparatus. Atomic absorption spectrophotometer (AAS) or inductively coupled plasma optical emission spectrometry (ICP-OES) was used for the detection of iron and its inorganic oxide.@*Results@#The sampling efficiency was higher than 97%; under the 372.0 nm wavelength, the linearity of AAS was good at the range of 1.0~150.0 μg/ml, the minimum quantitation concentration was 0.28 mg/m3, the maximum quantitation concentration was 6.24 mg/m3, the recovery was ranged from 99%~102%, the RSD of intra-and inter-batch precision were 0.5%~1.2% and 1.0%~2.2%, respectively; the linearity of ICP-OES was good at the range of 0.1~500 μg/ml, the minimum quantitation concentration was 0.28 mg/m3, the maximum quantitation concentration was 20.8 mg/m3, the recovery was ranged from 101%~103%, the RSD of intra-and inter-batch precision were 0.5%~1.0% and 1.5%~1.6%, respectively.@*Conclusion@#The sampling method and determination method meet the requirements of analysis and apply to the collection and determination of iron and its inorganic oxide in the air of workplace.
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Objective@#To establish ion chromatography method to determine thiocyanate within urine of workers who were exposed to cyanide.@*Methods@#After the workers work, used 50 ml centrifuge tube to collect the urine of workers about 20 ml.The urine were tested by centrifugation, dilution and filtration by C18 column, thiocyanate was separated by AS16 and mobile phase elution by KOH, detected by electrical circuitryconductivity detector, quantitative by the standard curve method.@*Results@#The linear correlation coefficient of thiocyanate within the range of 0.1-5.0 μg/ml was more than 0.999. The method detection limit was 0.11μg/ml (in 1ml urine) , the method quantitative limit was 0.35 μg/ml. The method recoveries were 95.1%-99.7%. The within-day precision range was 0.54%-2.05%, The between-run precision range was 2.06%-5.09%. Sample stability test showed that thiocyanate samples could be stored for 5 days at room temperature and 7 days at 4 ℃, could be stored for 14 days at-20 ℃.@*Conclusion@#The technical indicator of method compliance with rule of Guide for establishing occupation health standards-Part 5: determination methods of chemicals in biological materials (GBZ/T 210.5-2008) , the method applies to workers who were exposed to cyanide.
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<p><b>OBJECTIVE</b>To describe the distribution of zinc (Zn) and copper (Cu) in urine samples of generalpopulation in eight provinces of China, to analyze their characteristics of distribution between different region, gender and age-cohorts, and to provide the baseline of themetabolites in the general population.</p><p><b>METHODS</b>From 2009 to 2010, 18 120 subjects from the general population aged from 6 to 60 years old were recruited from 24 areas among 8 provinces of China mainland by random sampling. The environmental and physical condition characteristics were collected from questionnaires, and urine samples were collected at the mean time. The levels of Zn and Cu in urine were measured using ICP-MS. Data were analyzed by statistical methods to compare the distribution characteristics of Zn and Cu among populations with different ages and genders.</p><p><b>RESULTS</b>Totally, the median of Cu and Zn in urine were 9.28 and 115.47 µg/L respectively; and the inter-quartile range of Cu and Zn were 2.66-16.09 and 35.32-265.15 µg/L respectively. The median of Cu in male and female were 9.90 and 8.60 µg/L (Z=-5.63, P<0.001), and Zn in male and female were 140.44 and 95.27 µg/L (Z=-14.79, P<0.001). The median of Cu among the groups aged 6-12, 13-16, 17-20, 21-30, 31-45 and 46-60 years old were 9.30, 10.14, 9.67, 9.33, 8.38 and 8.74 µg/L (χ2=70.94, P<0.001), respectively, and the median of Zn 130.83, 132.07, 139.34, 109.3, 78.74 and 109.51 µg/L ((χ2=146.00, P<0.001), respectively.There was statistically significant differences in urinary Cu and Zn levels between male and female, and among the different age groups.</p><p><b>CONCLUSION</b>The Cu and Zn levels and distribution in urine among general population between 2009 and 2010 in China were reported in this article. These basic data in China will provide scientific and reliable reference for further scientific research.</p>
Subject(s)
Adolescent , Adult , Child , Female , Humans , Male , Middle Aged , Age Factors , China , Copper , Urine , Environment , Sex Factors , Surveys and Questionnaires , Zinc , UrineABSTRACT
<p><b>OBJECTIVE</b>To establish a method for determination of N-isopropylaniline in the workplace atmosphere by gas chromatography.</p><p><b>METHODS</b>Air samples were collected by silica gel tube and desorbed by acetone. Then they were separated through DB-WAX columns and N-isopropylaniline was determined by flame ionization detector.</p><p><b>RESULTS</b>The concentration of N-isopropylaniline showed a good linear relationship within the range of 1.40∼665.0 µg/ml. The sampling efficiency was 100%. The accuracy was 96%∼ 99% and the precision was 2.1%∼7.0%. The minimum detectable concentration was 0.056 mg/m(3) (with sampled air volume of 7.5 L).</p><p><b>CONCLUSION</b>The method meets the requirements of analysis and applies to the determination of N-isopropylaniline in the workplace atmosphere.</p>
Subject(s)
Air , Air Pollutants, Occupational , Aniline Compounds , Chromatography, Gas , Methods , WorkplaceABSTRACT
<p><b>OBJECTIVE</b>To investigate the level of zinc (Zn) and copper (Cu) in whole blood among general population from 8 provinces in China, and to analyze the characteristics of distribution among different regions.</p><p><b>METHODS</b>This cross-sectional study was performed in 8 provinces from eastern, middle and western China between 2009 and 2010, including 13 110 subjects from 24 regions, and the blood and urine samples were collected. The ICP-MS was applied to test the content of ICP-MS in blood samples, and the results were used to analyze the characteristics of contents and distributions of Zn and Cu among population from different ages, genders and regions groups.</p><p><b>RESULTS</b>Totally, the mean (95%CI) contents of Cu and Zn in blood were 795 (791-799)µg/L and 3 996(3 976-4 015) µg/L, respectively. The characteristics of distribution of Cu content were as followed, the content of males were lower than it of females (male:767 µg/L; female: 822 µg/L, t = -13.302, P < 0.01). The contents of blood Cu in groups of people aging 6-12, 13-16, 17-20, 21-30, 31-45 and 46-60 years old were separately 860(853-868), 758(748-769), 734(728-734), 782(774-790), 811(795-827) and 820(815-826) µg/L. The differences showed statistical significance (F = 78.77, P < 0.01). The blood Cu content of people in eastern China (800µg/L) were also significantly higher than it in middle (774 µg/L)and western China (782 µg/L) (F = 10.94, P < 0.01). Distribution of blood Zn content showed characteristics as follows: the Zn content was higher in males than in females (male 4 085 µg/L and female 3 908 µg/L, t = 8.78, P < 0.01). The contents of blood Zn in groups of people aging 6-12, 13-16, 17-20, 21-30, 31-45 and 46-60 years old were separately 3 306 (3 261-3 350), 3 888 (3 839-3 937), 3 948 (3 902-3 994), 4 272(4 228-4 315), 4 231(4 180-4 281) and 4 250 (4 205-4 294)µg/L, which showed significant statistical differences (F = 233.68, P < 0.01). The blood Zn content of people in eastern China (3 938 µg/L) were significantly lower than it in middle (4 237 µg/L)and western China (4 105 µg/L) (F = 53.16, P < 0.01). In addition, the study also compared the relation between content of Cu and Zn and the frequency of eating seafood. The results found that the frequency of eating seafood could influence the content of Cu and Zn (Cu: F = 13.54, P < 0.01; Zn: F = 200.20, P < 0.01).</p><p><b>CONCLUSION</b>The contents and distributions of Cu and Zn in blood differs among people from different groups in ages, genders and regions. The baseline data of this study provided reliable scientific evidence for further research.</p>