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Objective Study on the stability of carbofuran and its metabolite carbofuran phenol in blood preserved at different conditions,in order to provide a scientific evidence for forensic identification of carbofuran poisoning death. Methods The dogs were given intragastric administration with 4LD50(13.5mg/kg) of carbofuran, the blood were collected and divided into five equally groups preserved at 20℃(NC2.5mg/mL), 20℃(1%NaF), 20℃, 4℃ and -20℃, respectively. The concentrations of carbofuran and carbofuran phenol in above samples were detected by GC-MS/MS with MRM at 0d、5d、7d、15d、40d、83d and 150d. Results The concentration of carbofuran in preserved blood were found to be significant decrease at 7d(P < 0.05), then a steady decline. In each condition, the concentration of carbofuran phenol in preserved blood showed an increasing trend firstly, then a declined tendency. The concentration of carbofuran and carbofuran phenol descending fast in blood at 20 ℃ (NC) and 20 ℃ (1%NaF).Conclusion Carbofuran and carbofuran phenol in preserved specimens are found to be decomposed. The decomposition is quick at 20℃ and slow at -20℃. Citrate sodium and sodium fluoride are not suit for anticoagulation and antiputrefactiva. Biological specimens used for forensic identification of the carbofuran poisoning should be stored at refriferated or freezed, and be analyzed as soon as possible.
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Objective To establish a kind of simple,rapid,accurate and reliable method to analyze the concentration of alcohol in blood by headspace gas chromatography (HS-GC) with dual-column and dual-detector.Methods The samples were pre-treated by headspace sampler,which was the basis on the extraction principle of the gas extracting volatile substances.Next,these samples were analyzed by HS-GC that the tertiary butyl alcohol was acted as the internal standard substance.The HS-GC was equipped with two chromatographic column (the DB-ALC2 chromatographic column of 001 channel;the DB-ALC1 chromatographic column of 002 channel).At the same time,the HS-GC was also equipped with two hydrogen flame ionization detector (FID1 detector;FID2 detector).The retention time of the peak was finally performed as qualitative parameter and the standard curves method of internal standard were acted as quantitative basis.Results The liner range of the method was 0.2-2.0 mg/mL.The linear regression equation of 001 channel was Y=1.057 7X+0.048 2 and the correlation coefficient was R2=0.999 05.Besides,the linear regression equation of 002 channel was Y=1.039 5X+0.046 5 and the correlation coefficient was R2=0.999 25.In short,the average recovery rate of the method was 99.70%.Relative standard deviation(RSD) was less than 4% between the analysis results of 001 channel and 002 channel for the determination of the plan sample.Conclusion The method shown satisfactorily that it could not only be applied to determine the alcohol of blood of forensic toxicological analysis,but also be applied to determine the plan sample of ability test and verify of laboratory ability accreditation.
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Objective To establish a kind of simple ,rapid ,accurate and reliable method to determine the phenobarbital in the biomaterial .Methods We pre‐treated biomaterial by the method that the reagent of acetone∶water (v/v 8∶2) was firstly used to soak the biomaterial ,and then we took use of ethyl acetate as reagent to extract the phenobarbital of the biomaterial in the present of pH=3-4 .We finally employed GC‐MS to determine these samples .On the one hand ,we not only took advantage of the reten‐tion time of the phenobarbital in total ion current (TIC) but also took advantage of the characteristic fragment ions of phenobarbital in mass spectrogram as qualitative basis .On the other hand ,we took advantage of the external standard method as quantitative ba‐sis .Results The method had the characteristics of the simple and easy operation .There was hardly background interference and there was good separation effect in the method .The method also had the characteristics of fast analytical speed such as the retention time of the phenobarbital was 8 .385 min .The characteristic fragment ions of phenobarbital was m/z 204 and m/z 232 .The charac‐teristic fragment ions of m/z 204 was served as quantitative ion fragments and we employed the external standard method to quanti‐fy in the method .In short ,the average recovery rate of the method was 87 .35% .Relative standard deviation (RSD) was 5 .43% in the method .The lowest limit of detection (LLOD) was 0 .005 mg/mL .Conclusion The method showes satisfactory result that it could be applied to determine the phenobarbital of the biomaterial of forensic toxicological analysis .
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Objective The study aimed to establish a kind of simple,rapid,accurate and reliable method in order to simultaneous determine the phenobarbital,ibuprofen and nikethamide in the biomaterial. Methods The biomaterial were pre-treated with ethanol(v/v 95%)at pH 3~4 and then was extracted with ethyl acetate at pH 3~4 and 10~11,respectively. Finally,phenobarbital,ibuprofen and nikethamide in the biomaterial were simultaneous detected by GC-MS. The retention times and relevant characteristic fragment ions of the three substances in the total ion current(TIC)and the mass spectrogram could be used as the basis of qualitative analysis. Results The method was simple and easy operation. It has the characteristics of low background interference,good separation effect and fast analytical speed. The retention times of phenobarbital,ibuprofen and nikethamide were 8.472 min,7.087 min and 6.655 min,respectively. The characteristic fragment ions of phenobarbital were 204 and 232(m/z),of ibuprofen were 161 and 206(m/z),and of nikethamide were 106 and 177(m/z). Conclusion The method showed a satisfactory result that it could be applied to simultaneous determine phenobarbital,ibuprofen and nikethamide of the biomaterial for forensic toxicological analysis.
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Objective To develop a method for the determination of ganciclover in human plasma by RPHPLC.Methods Plasma containing ganciclover was extracted with methanol and methylene chloride,qualitative and quantitative analysis was carried out directly.Working curve,linear range,recovery,precision and so on was obtained according to the sample pre-processing method and analysis state.The HPLC method has been taken to investigate the plasma concentration of ganciclover for 12 volunteers.Results The relationship of the peak area of ganciclover concentration in plasma linear within the range of 0.05 μg/mL～1.60 μg/mL(r=0.9999).The lowest detection limit was 0.01 μg/mL(S/N≥13).The intra and inter-day RSD were less than 5.1%respectively.The recovery is about 90.0%～95.4%.Conclusion The established method in the article was shown to be sensitive,accurate and simple for the determination of ganciclover level.It is suitable for clinical detection of ganciclover and forensic medicine and toxicology analysis.
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Objective A method for the determination of 4-methylimidazole in soy sauce by capillary gas chromatography was studies.Methods The method consisted of a methylene chloride to elution,followed by concentration of the eluate.N,N-Dimethylaniline(IS) was added in and GC analysis of the eluate,prior to GC analysis.The GC analysis was carried out by DB-FFAP capillary column and nitrogen phosphorus detector(NPD).Results The linear range was 4.9mg~1.5?102 mg/L and the limit of detection was 0.16 ug/L.The average recoveries were 97.25%and 99.44% by stand addition method in 0.0102mg and 0.0602mg 4-methylimidazole.Conclusion The method was simple,rapid and sensitive.A useful method for determining 4-methylimidazole in soy sauce was provided for forensic analysis.
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Objective To develop a method for simultaneous determination of benzodiazepines in human whole blood by SPE-Micellar electrokinetic capillary chromatography.Methods With the Clenbuterol as internal standard,Oasis column was used to extract the drugs from whole blood.The separation was performed on a fused-silica capillary of 75?m ID?50.2cm(40cm of effect length).The running buffers were sequentially used as 15mmol/L phosphates→15mmol/L sodium borate(pH8.2)→30 mmol/L SDS,and 18% methanol served as an organic modifier.Sample solution was injected with pressure mode,and the running voltage was 25kV.The detection wavelength was set at 230nm.Results The linear ranges of the calibration curves were from 0.02 to 1.6?g/ml,and the limits of detection ranged between 5 ng/ml and 50 ng/ml.The within-day and between-day precision was less than 12%.Conclusion The method developed for determination of benzodiazepines in human whole blood is effective,simple and reliable,with which 9 benzodiazepines may be simultaneously separated.