Objective To investigate the association between rheumatoid arthritis (RA) and the presence of the shared epitope (SE) of HLA DRB1 gene in Han nationality of Shandong population.Methods The method of DNA amplification with sequence specific primers (PCR SSP) was used to determine 17 alleles of HLA DRB101,04,10 genotypes in 132 RA patients and 130 healthy controls from the Han nationality population in Shandong.Results The frequencies of SE were significantly increased in RA patients compared with controls (50 0% vs 22 3%, P

Objective:To explore the relationship of CDH17 expression with clinico-pathological features and the correlation be-tween the single nucleotide polymorphisms (SNPs) of CDH17 gene and genetic susceptibility of gastric carcinoma (GC). Methods:A tissue microarray was performed to simulate the dynamic process of invasion and metastasis of GC. Immunohistochemical staining was performed to detect the expression of CDH17 protein, and PCR-based LDR was performed to detect the 2 SNP loci (rs2514813 and rs3214050) genotypes of CDH17 gene. Results: The expression of CDH17 protein in GC was more significantly up-regulated and greatly increased in the intestinal type than in the diffuse type. The expression of CDH17 protein in GC was positively correlated with the histological grading (P<0.01) and was not associated with the survival (P=0.209). With the progression of the cancer invasion, the expression of CDH17 protein in GC showed a downtrend from the gastric mucosa layer to the invasive front edge. The frequencies of the C and T alleles and the CC, CT, and TT genotypes at the CDH17 rs3214050 locus between the GC patients and the control groups were significantly different (P<0.01). However, no significant differences were observed at rs2514813 (P>0.05). The individuals with the T al-leles had longer survival time than those with the CC genotype (P<0.01). Conclusion:The up-regulation of CDH17 expression is in-volved in the maintenance of histological phenotype and progression of GC. Individuals with T alleles at the CDH17 rs3214050 locus have decreased risk of GC and had better prognosis (OR=0.762, 95%CI:0.619-0.937), thereby suggesting that screening for these alleles would help with the assessment of genetic susceptibility and prognosis of GC in the Fujian population.

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.

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.

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.

OBJECTIVETo establish a method for determination of N-isopropylaniline in the workplace atmosphere by gas chromatography.

METHODSAir 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.

RESULTSThe 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).

CONCLUSIONThe method meets the requirements of analysis and applies to the determination of N-isopropylaniline in the workplace atmosphere.

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.

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.

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.

A rapid analysis method based on ultraviolet-visual(UV-Vis) spectroscopy, near infrared(NIR) spectroscopy and multivariable data analysis was established for quality evaluation of Shengxuebao Mixture. The contents of eight active ingredients of Shengxuebao Mixture including albiflorin, paeoniflorin, 2, 3, 5, 4'-tetra-hydroxy-stilbene-2-O-β-D-glucopyranoside, specnuezhenide,ecliptasaponin D, emodin, calycosin-7-glucoside and astragaloside Ⅳ were simultaneously detected by using this method. HPLC-UV-MS was used as a reference method for determining the contents of these ingredients. Partial least squares(PLS) analysis was implemented as a linear method for multivariate models calibrated between UV spectrum/NIR spectrum and contents of 8 ingredients. Finally, the performance of the model was evaluated by 24 batches of test samples. The results showed that both UV-Vis and NIR models gave a good calibration ability with an R~2 value above 0.9, and the prediction ability was also satisfactory, with an R~2 value higher than 0.83 for UV-Vis model and higher than 0.79 for NIR model. The overall results demonstrate that the established method is accurate, robust and fast, therefore, it can be used for rapid quality evaluation of Shengxuebao Mixture.
Calibration ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; Least-Squares Analysis ; Mass Spectrometry ; Spectroscopy, Near-Infrared