Objective:To establish a method for the determination of 2, 3-Butanedione (BUT) in the air of workplace, which including the process of collection by absorption in phosphoric acid aqueous solution and the process of analysis and detection by high performance liquid chromatography with derivatization.Methods:In October 2022, a porous glass plate absorption tube containing 10 ml of 0.01% phosphoric acid solution was used to collect BUT in the air of the workplace at a flow rate of 0.2 L/min. The absorption solution was derived by 2, 4-dinitrophenylhydrazine for 75 min and separated on a SB-C18 column (250 mm×4.6 mm, 5 μm) . At the column temperature of 30 ℃, the mixture of acetonitrile-water ( V∶ V, 1∶1) was eluted at the flow rate of 1.0 ml/min. It was detected by UV detector (λ=365 nm) , qualitatived by retention time and quantitatived by external standard. Results:It showed that BUT in phosphoric acid aqueous solution could be stored for at least 7 d at 4 ℃. There was a linear relationship within the determination range of 0.05-6.00 μg/ml, the linear regression equation was y=89.610 x+0.133, r=0.9999. The sampling absorption efficiencies were 98.33%-100.00%, the detection limit of the method was 0.005 μg/ml, the minimum detection concentration was 0.016 mg/m 3 (based on V0=3.0 L) . The recovery rates were 95.96%-102.44%, the intra batch precision were 4.36%-7.78%, and the inter batch precision were 4.96%-6.06%. Conclusion:The method has the advantages of simple operation, high sensitivity and good accuracy. It can prevent the loss and degradation of BUT. It can be used for the determination of BUT in the air of workplace.

Objective:To establish a method for the determination of 2, 3-Butanedione (BUT) in the air of workplace, which including the process of collection by absorption in phosphoric acid aqueous solution and the process of analysis and detection by high performance liquid chromatography with derivatization.Methods:In October 2022, a porous glass plate absorption tube containing 10 ml of 0.01% phosphoric acid solution was used to collect BUT in the air of the workplace at a flow rate of 0.2 L/min. The absorption solution was derived by 2, 4-dinitrophenylhydrazine for 75 min and separated on a SB-C18 column (250 mm×4.6 mm, 5 μm) . At the column temperature of 30 ℃, the mixture of acetonitrile-water ( V∶ V, 1∶1) was eluted at the flow rate of 1.0 ml/min. It was detected by UV detector (λ=365 nm) , qualitatived by retention time and quantitatived by external standard. Results:It showed that BUT in phosphoric acid aqueous solution could be stored for at least 7 d at 4 ℃. There was a linear relationship within the determination range of 0.05-6.00 μg/ml, the linear regression equation was y=89.610 x+0.133, r=0.9999. The sampling absorption efficiencies were 98.33%-100.00%, the detection limit of the method was 0.005 μg/ml, the minimum detection concentration was 0.016 mg/m 3 (based on V0=3.0 L) . The recovery rates were 95.96%-102.44%, the intra batch precision were 4.36%-7.78%, and the inter batch precision were 4.96%-6.06%. Conclusion:The method has the advantages of simple operation, high sensitivity and good accuracy. It can prevent the loss and degradation of BUT. It can be used for the determination of BUT in the air of workplace.

Background Diacetyl (DC) is widely used in the food flavoring industry and excessive occupational exposure to DC can cause serious respiratory diseases. However, there is no corresponding national standard method for the determination of DC in the air of workplace. Objective To establish a method for the determination of DC in workplace air by high performance liquid chromatography using 4-nitro-o-phenylenediamine (NPDA) as precolumn derivatization. Methods DC in the air of workplace was collected by solution absorption method. This experiment used NPDA as the derivatization reagent. By adjusting acidity of solution and optimizing concentration ration of DC/NPDA, derivatization temperature, and time, a method for the determination of DC in workplace air was proposed, and its performance indexes such as linearity, detection limit, and lower limit of quantification were obtained. Sampling efficiency was evaluated by relative comparison method, and sample stability was evaluated by sample preservation test. Accuracy and precision of the method were evaluated by standard addition recovery test with blank samples, and an interference test was carried out by adding standard samples. The established method was applied to actual samples to evaluate its adaptability. Results A combination of 60 °C for 2 h was selected for derivatization because a higher derivatization reaction temperature and a longer reaction time associated with a higher derivatization efficiency. The solution was separated by SB-C18 column (250 mm×4.6 mm, 5 μm) at 30 ℃, using a mixture of methanol and water (v/v, 65%/35%) as mobile phase with an elution flow rate of 1.0 mL·min⁻¹, and was detected with a variable wavelength detector (λ_max=257 nm) by qualitative analysis based on retention time and quantitative analysis based on external standard method. In terms of the proposed method, the linear range of detection was from 5 μg·L⁻¹ to 2000 μg·L⁻¹, with a correlation coefficient of 0.9999, and a detection limit of 1.3 μg·L⁻¹, the quantitative detection of the lower limit was 4.3 μg·L⁻¹, with a sampling volume V₀ of 3.0 L, the minimum detection concentration was 4.3 μg·m⁻³, and the minimum quantitative concentration was 14.3 μg·m⁻³. The recovery rate was 99.1%-100.8%, the intra-batch precision was 0.5%-3.0%, and the inter-batch precision was 1.2%-2.0%. The average sampling efficiency of this method was 94.5%, and the sample could be stored at 4 °C for at least 14 d. The coexisting components in the air of the workplace did not interfere with the determination of DC. The DC content in the air of a flavor workplace was 5.86-8.85 mg·m⁻³. Conclusion A determination method for DC in workplace air by high performance liquid chromatography using NPDA as precolumn derivatization after being collected by 1.0% phosphoric acid absorbent is proposed and has the advantages of simple operation, high sensitivity, and good accuracy. With no DC loss and degradation, the method may satisfy the request for DC determination in the air of workplace.

Objective:To explore the performance of the commonly used whole blood C-reactive protein (CRP) detection systems and give related recommendation on the performance requirements of detection systems.Methods:A total of 7 540 venous blood samples from 26 maternal, child and children′s hospitals were collected to conduct this multi-center study on the analytical performance of 5 commonly used whole blood CRP detection systems from March to April in 2019. The blank check, carryover, repeatability, intermediate precision, linearity, sample stability, influence of hematocrit/triglyceride/bilirubin, comparison with SIEMENS specific protein analyzer and trueness were evaluated. The 5 systems included BC-5390CRP autohematology analyzer, AstepPLUS specific protein analyzer, Ottoman-1000 Automated Specific Protein POCT Workstation, i-CHROMA Immunofluorometer equipment Reader and Orion QuikRead go detecting instrument. The 5 systems were labeled as a, b, c, d and e randomly.Results:Within the 5 systems, all values of blank check were less than 1.00 mg/L, the carryovers were lower than 1.00%. The repeatability of different ranges of CRP concentrations including 3.00-10.00, 10.00-30.00 and>30.00 mg/L were less than 10.00%, 6.00% and 5.00%, respectively, and the intermediate precision was less than 10.00%. The linearity correlation coefficients of the 5 systems were all above 0.975, while the slope was within 0.950-1.050. Whole blood samples were stable within 72 hours both at room temperature (18-25 ℃) and refrigerated temperature (2-8 ℃). The CRP results were rarely influenced by high triglyceride or bilirubin, except for the immmunoturbidimetric test based on microparticles coated with anti-human CRP F(ab) 2 fragments. When triglyceride was less than 15.46 mmol/L, the deviation of CRP was less than 10.00%. When bilirubin was less than 345.47 μmol/L, the deviation of CRP was less than 10.00%. CRP was more susceptible to Hct on the systems without Hct correction. The deviation of CRP between different Hct dilution concentration and 40% dilution concentration can reach as high as 67.48%. The correlation coefficients ( r) of 5 systems were all more than 0.975 in the range of 0-300.00 mg/L compared with Siemens specific protein analyzer. All systems passed the trueness verification using the samples with specified values of 12.89 and 30.60 mg/L. Conclusion:The performance of 5 systems can basically meet the clinical needs, but it is suggested that the whole blood CRP detection system without automatic Hct correction should be modified manually.

Objective:To establish a method for determination of the butanone in urine by gas chromatography (GC) with pre-column derivation.Methods:For detecting of butanone in urine, potassium iodide and potassium dichromate were added into urine under acidic condition, sample derivatization was undertaken in 50 ℃ water bath for 60 min and the iodine butanone was extracted with n-hexane. After the sodium thiosulfate solution was used to remove excess iodine, urine samples were centrifuged at 10000 r/min for 5 min, then the supernatant was analyzed using temperature rising programming with the Agilent Hp-5 column (30 m×0.32 mm, 0.25 μm) and electron capture detector (ECD) as the detector. The detector temperature was 300 ℃, the inlet temperature was 200 ℃, and the carrier gas was nitrogen.Results:For detecting of butanone in urine, potassium iodide and potassium dichromate were added for derivatization under the acidic condition. After extraction and centrifugation, the supernatant directly put through column and detected by ECD. In present study, the sample pretreatment condition was optimized, the relative standard deviations of intra-day and inner-day, the spiked samples and its recovery were evaluated for analyzing the accuracy of the proposed method.Conclusion:This method has proved to be simple, efficient and highly sensitivity, it can be utilized for butanone detection in occupational population.

Objective:To establish a method for determination of the butanone in urine by gas chromatography (GC) with pre-column derivation.Methods:For detecting of butanone in urine, potassium iodide and potassium dichromate were added into urine under acidic condition, sample derivatization was undertaken in 50 ℃ water bath for 60 min and the iodine butanone was extracted with n-hexane. After the sodium thiosulfate solution was used to remove excess iodine, urine samples were centrifuged at 10000 r/min for 5 min, then the supernatant was analyzed using temperature rising programming with the Agilent Hp-5 column (30 m×0.32 mm, 0.25 μm) and electron capture detector (ECD) as the detector. The detector temperature was 300 ℃, the inlet temperature was 200 ℃, and the carrier gas was nitrogen.Results:For detecting of butanone in urine, potassium iodide and potassium dichromate were added for derivatization under the acidic condition. After extraction and centrifugation, the supernatant directly put through column and detected by ECD. In present study, the sample pretreatment condition was optimized, the relative standard deviations of intra-day and inner-day, the spiked samples and its recovery were evaluated for analyzing the accuracy of the proposed method.Conclusion:This method has proved to be simple, efficient and highly sensitivity, it can be utilized for butanone detection in occupational population.

Objective To evaluate different methods in detecting intraperitontal free cancer cells (IFCCs) in patients with gastric cancer and to clarify the relationship between positive IFCCs and short-term prognosis.Methods A total of 119 gastric cancer patients who underwent surgical treatment were enrolled.Peritoneal lavage was performed with 300-400 ml saline respectively at three points of time:immediately after abdominal cavity entry;when surgical operation was completed;when extensive intraoperative peritoneal lavage was done.The IFCCs were detected with methods of traditional centrifugal cytology,membrane cytology,ICC and RT-PCR.The survival curve of patients with gastric cancer was drawn using Kaplan-Meier method.Results The positive rate of PLC was 16.8％,20.7％ and 11.2％ respectively at 3 timepoints (P ＜ 0.05).The positive rates of ICC were 28.6％,38.8％ and 20.7％ respectively at 3 timepoints.The positive rates of RT-PCR were 39.3％,69.5％ and 50.8％ respectively at 3 time points.The positive rate of IFCCs detected through RT-PCR was higher than that of PLC and ICC (P ＜ 0.05).The short-term prognosis of patients with positive IFCCs was worse than those with negative results detected with any three method at the timg point immediately after opening the abdomen (P ＜ 0.05).At the timg point immediately after removing the tumors,the short-term prognosis of patients with positive IFCCs detected with PLC was worse (P ＜ 0.05).Conclusion The short-term prognosis was poor in patients with positive IFCCs.It is the best time to detect IFCCs before radical resection.Surgical procedures increase the risk of shedding of IFCCs.

Objective: To establish a method for determination the S-phenylmercapturic acid in urine by dispersive solid-phase extraction using Humic Acid/Fe₃O₄ magnetic nanocomposite as adsorbent. Methods: The 5 ml of urine samples were adjusted to pH 1.0 and extracted by Fe3O4@HA. Then the analytes were separated on EC-C₁₈ capillary column and detected by HPLC-VWD. The S-phenylmercapturic acid was characterized by the retention time and quantified by peak area and external standard method. Results: The standard curves of SPMA showed significant linearity between 0.04~1.00 mg/L (r=0.999 7) . The average recovery was 94.2%~102.4%. The intra-day and inter-day precisions (RSD) were 2.9~6.7% (n=6) and 3.1~7.5% (n=6) respectively. The detect limit of SPMA was 0.012 g/L (S/N=3) . Conclusion This method is simple, rapid, sensitive and accurate. It is applicable for determination of SPMA in the urine of works who were exposed to benzene.

Objective: To establish a method for determing the trichloroethylene(TCE)and trichloroethanol(TCOH)in blood samples by liquid-liquid extraction-gas chromatography with electron capture detector. Methods: With this method,ether was used as extraction solvent and trichloromethane was used as an internal standard. The whole blood sample was extracted with ether, and dehydrated by anhydrous sodium sulfate. Then the analytes were separated on HP-5 capillary column(30m×0.32mm×0.15μm)and detected byECD.The retention time was for qualitative analysis and the internal standard was for quantitation. Results: The standard curves of TCE and TCOH showed significant linearity between 95.5μg/L-7640.0μg/L(r=0.9997)and 19.0μg/L-1520.0μg/L(r=0.9992). The average recovery was 95.5%-103.6%.The intra-day and inter-day precisions(RSD)were 2.5%-6.8%(n=6)and 1.6%-4.3%(n=6) respectively. The detect limit of TCE and TCOH were 2.10 μg/L and 0.56μg/L(S/N=3)respectively.The blood can be kept 7 days at-20℃ refrigerator without significantly loss. Conclusion This method is proved to be simple,practical and highly sensitive. It can satisfy the request for the determination of blood samples of humans exposed to TCE.

To investigate hematopoiesis and cytogenetics changes in staff of interventional radiology.A total of 121 intervention radiation workers, 245 common radiation workers and 100 medical personnel (healthy control) without exposure to radiation were enrolled in the study. The peripheral lymphocyte chromosomal aberrations and micronucleus were detected, and the result of white blood cells examination was analyzed.Compared with common radiation group and healthy control group, decreases in white blood cells count, neutrophil ratio, and increase in lymphocyte ratio were observed in intervention radiation group (all<0.05). Intervention radiation group had higher chromosome aberration rate and micronuclear rate than common radiation group and healthy control group (all<0.05). Most common chromosome aberrations were dicentric chromosome, acentric ring, fragments and minute chromosome. Abnormal rates in chromosome aberration and micronucleus rates were increased with the rise of length of service, but no statistically significant difference was observed (>0.05).Long term exposure to ionizing radiation may lead to changes in the human hematopoietic system and cause human chromosome aberration, and the severity of such injuries may be associated with the dose of ionizing radiation.
Adult ; Chromosome Aberrations ; radiation effects ; Dose-Response Relationship, Radiation ; Female ; Hematopoiesis ; radiation effects ; Humans ; Leukocyte Count ; statistics & numerical data ; Leukocytes ; pathology ; radiation effects ; Lymphocytes ; pathology ; radiation effects ; ultrastructure ; Male ; Micronuclei, Chromosome-Defective ; radiation effects ; Occupational Exposure ; adverse effects ; Radiation Exposure ; adverse effects ; statistics & numerical data ; Radiation, Ionizing ; Radiologists ; statistics & numerical data ; Time Factors