Biological desulfurization is a process in which sulfur compounds are removed from gas and oil using microorganisms. It is a simple process that has mild operating conditions, high desulfurization efficiency, low energy consumption and less environmental pollution. However, there is still a lack of simple and efficient analytical methods for quantitatively analyzing the sulfur compounds in the biological desulfurization process. In order to solve this problem, the analytical method for the simultaneous determination of sulfite, thiosulfate and sulfide in biological desulfurization solutions by pre-column fluorescence derivation using high performance liquid chromatography (HPLC) was developed. The standard curves of sulfur species in this analytical method had good linear relationships with correlation coefficients of 0.999 5, 0.999 7, and 0.999 7 for sulfite, thiosulfate and sulfide, respectively. The detection limits of these sulfur compounds were 0.000 6, 0.000 7 and 0.001 1 μmol/L; the range of recovery rates were 98.17 to 101.9%, 100.9 to 102.6%, and 101.1 to 104.2%; which had good repeatability and stability. The analytical method was simple, efficient and accurate, and could be used to simultaneously determine the sulfur compounds in different biological desulfurization systems.
Chemistry Techniques, Analytical/methods* ; Chromatography, High Pressure Liquid ; Sulfur Compounds/analysis*

Objective To provide the reference for the identification of unknown fentanyl analogues by studying the characteristic ions and main fragmentation pathways of fentanyl analogues in the modes of collision induced dissociation （CID） and electron ionization （EI）. Methods Nine fentanyl analogues （2, 2'-difluorofentanyl, acetyl fentanyl, fentanyl, butyl fentanyl, valeryl fentanyl, acryloyl fentanyl, furan fentanyl, 4-fluorine isobutyl fentanyl, carfentanyl） were selected and analyzed with ultra-high performance liquid chromatography-quadrupole time-of-flight-mass spectrometry （UHPLC-QTOF-MS） and gas chromatography-mass spectrometry （GC-MS）. The mass spectrum obtained was analyzed. The CID and EI fragmentation routes of fentanyl analogues were speculated. Results The CID and EI fragmentation pathways were highly similar. In the CID mode, characteristic ions were formed by the carbon-nitrogen bond cleavage between the piperidine ring and the N-phenyl-amide moiety, within the piperidine ring, and between the phenethyl and piperidine ring. While in the EI mode, dissociation of the piperidine ring, as well as cleavage between the piperidine ring and the phenethyl were the main fragmentation pathways. Conclusion This study summarizes the main fragmentation pathways and characteristic ions of fentanyl analogues in the CID and EI modes, which is useful for forensic laboratories to identify and structural analyze fentanyl type new psychoactive substance in practical work.
Chemistry Techniques, Analytical/methods* ; Chromatography, High Pressure Liquid ; Fentanyl/analysis* ; Gas Chromatography-Mass Spectrometry ; Humans ; Mass Spectrometry

OBJECTIVE: : To analyze experimental factors affecting recovery of puerarin in microdialysis. METHODS: : Puerarin concentration in microdialysate samples was determined by high performance liquid chromatography. The methods of direct dialysis, retrodialysis and the zero-net flux were used to calculate recovery, respectively. The effects of perfusate composition, the analyte concentration, perfusate flow rate, medium temperature and stir rates of the dialysis medium on recovery were investigated. RESULTS: : There were significant differences in the recovery values among direct dialysis, retrodialysis and zero-net flux methods. The recovery for 0.9% NaCl solution, Ringer's solution, PBS and anticoagulant dextrose solution as perfusate fluid were (71.25±2.36)%,(73.48±1.41)%,(68.50±2.43)% and (74.98±1.16)%, respectively. The composition of perfusate fluid had significant influence on the recovery(<0.01). At the same flow rate, recovery was independent of the analyte concentration. At the same concentration, the recovery was decrease with the increasing flow rate in an exponential relationship. The recovery increased with the raising temperature and stir rate of the dialysis medium, and the recovery remained stable when the stir rate reached above 200 rpm. CONCLUSIONS : A study method for recovery of puerarin in microdialysis has been established, and the recovery of puerarin is affected by calculating methods, perfusate fluids, flow rate, medium temperature and stir rate, but not affected by analyte concentrations.
Chemistry Techniques, Analytical ; methods ; Chromatography, High Pressure Liquid ; Isoflavones ; isolation & purification ; Microdialysis

The present study was designed to establish a multi-wavelength quantitative fingerprinting method for San-Huang Tablets (SHT), a widely used and commercially available herbal preparation, where high performance liquid chromatography (HPLC) with a diode array detector (DAD) was employed to obtain the fingerprint profiles. A simple linear quantitative fingerprint method (SLQFM) coupled with multi-ingredient simultaneous determination was developed to evaluate the quality consistency of the tested samples qualitatively and quantitatively. Additionally, the component-activity relationship between chromatographic fingerprints and total radical-scavenging capacity in vitro (as assessed using the 1, 1-diphenyl-2-picrylhydrazyl (DPPH) assay) was investigated by partial least squares regression (PLSR) analysis to predict the antioxidant capacity of new samples from the chromatographic fingerprints and identify the main active constituents that can be used as the target markers for the quality control of SHT. In conclusion, the strategy developed in the present study was effective and reliable, which can be employed for holistic evaluation and accurate discrimination for the quality consistency of SHT preparations and other traditional Chinese medicine (TCM) and herbal preparations as well.
Antioxidants ; chemistry ; Biphenyl Compounds ; chemistry ; Chemistry Techniques, Analytical ; methods ; Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; chemistry ; Free Radicals ; chemistry ; Molecular Structure ; Picrates ; chemistry ; Quality Control ; Tablets ; chemistry

OBJECTIVETo compare the determination methods of fiber number concentration between China and WHO.

METHODSIndividual fiber samplings were conducted at a RCF manufacturing enterprise for 40 types of work. Flow rate was set as 2 L/min and lasted 2 to 4 hours. We used acetone-triacetin to prepare samples. The rules of two methods were used to count fibers for each sample respectively. The differences between the results of two methods were compared using the sign-rank test, and the correlation between the two methods' counting results were evaluated by the Spearsman rank correlation analysis.

RESULTSThe results of WHO counting rule were higher than those of Chinese counting rule for the same sample. The ratios of WHO method to Chinese method ranged from 1.88 to 3.70. Paired sign-rank test found the statistically significant differences of the results between the two methods (P<0.01). The rank correlation coefficient of the results by two rules counting ranged between 0.621 to 0.975, suggested positive correlation (P<0.01). The possible reasons of the difference between the two methods included the difference between the shapes of asbestos fiber and man-made mineral fiber, and counting rules of two methods.

CONCLUSIONThe results of WHO counting method is higher than those of Chinese counting method. High correlations between the results of the two methods were observed.

Asbestos ; analysis ; Chemistry Techniques, Analytical ; methods ; China ; Humans ; Mineral Fibers ; analysis ; Specimen Handling ; World Health Organization

High resolution melting (HRM), an important technology for genotyping and mutation scanning, has broad prospects in the authentification of traditional Chinese medicine. This paper selected universal trnH-psbA primers and used HRM to establish a new methods for identification of Akebia herbs. PCR was conduct at the annealing temperature of 58 degrees C and 35 cycles. The range of the DNA template concentration, the primer concentration and the Mg2+ ion concentration were further analyzed. The results showed the Tm values of Caulis Akebiae was (81.84 ± 0.16), (85.28 ± 0.16) degrees C and Caulis Clematidis Armandii was (83.22 ± 0.19) degrees C and Caulis Aristolochiae manshuriensis was (81.67 ± 0.14) degrees C, (84.24 ± 0.10) degrees C with 5-125 mg - L-' DNA template, 0.4 μmol x L(-1) primer, 2.0 mmol x L(-1) Mg2+. This method can achieve the authentification of Akebia herbs and is simple, fast, high-throughput, visual.
Chemistry Techniques, Analytical ; methods ; DNA, Plant ; chemistry ; genetics ; Genotype ; Magnoliopsida ; chemistry ; classification ; genetics ; Phylogeny ; Transition Temperature

Calibration ; Chemistry Techniques, Analytical ; methods ; Humans ; Lead ; blood

The content of SO2 in Paeoniae Radix Alba (RPA) was determined by the method documented in Chinese Pharmacopoeia (CP) 2010 edition to validate the repeatability of the method for evaluating RPA, and the contents of paeoniflorin sulfonate in both the residual material and distilled solution of RPA were determined by HPLC to study the transformation of paeoniflorin sulfonate to SO2 by HCl. It was found that the repeatability of the method in CP for evaluating RPA is unacceptable, and paeoniflorin sulfonate was detectable in both the residual material and distilled solution of RPA even at "the end point" of SO2 determination, merely about 50% of paeoniflorin sulfonate was transformed to SO2 by HCl, indicating that the current SO2 determination method in CP is not able to accurately quantify SO2 in RPA. It is recommended that more special method for determining SO2 content in RPA should be developed regarding the chemical characteristics of sulfur-fumigated RPA.
Chemistry Techniques, Analytical ; methods ; Chemistry, Pharmaceutical ; Drugs, Chinese Herbal ; analysis ; Fumigation ; Glucosides ; analysis ; Monoterpenes ; analysis ; Paeonia ; chemistry ; Pharmacopoeias as Topic ; standards ; Sulfur Dioxide ; chemistry

Study a method for the detemination of the content of polysaccharides in Gentiana farreri, and analysis of the content of polysaccharides from different producing areas. The results showed that using the anthrone-sulfuric acid method, simple operation, accurate result. Sample was measured at 620 nm absorbance after anthrone-sulfuric acid color, at this wavelength, solution absorption and glucose showed a good linear relationship; The linearity was in the range of 0.01-0.07 g x L(-1) (r = 0.996 7). The recovery rate was 99.41%, with RSD of 2.0%. Considering the experimental conditions, to determine the solid-liquid ratio 1:60, extracting time 50 min, concentration of ethanol 80%. The mass fraction of polysaccharides was the highest to reached 0.743% in G. farreri from Gansu Xiahe. This experiment has laid a good foundation for further study on G. farreri.
Anthracenes ; chemistry ; Chemistry Techniques, Analytical ; methods ; Gentiana ; chemistry ; growth & development ; Geography ; Linear Models ; Polysaccharides ; analysis ; Reproducibility of Results ; Sulfuric Acids ; chemistry ; Time Factors

Suitable pretreatment of biological samples can truly reflect the role of law of the measured components played in the body and will provide experimental evidence for the studies on metabolic process, material basis of efficacy, mechanism of action, pharmacology, toxicology and the others. Biological samples include blood, urine, hair, tears, etc. There are also many samples processing methods, such as the direct protein precipitation, liquid-liquid extraction and solid phase extraction and so on. These methods could be used alone or combined.
Animals ; Body Fluids ; chemistry ; Chemical Precipitation ; Chemistry Techniques, Analytical ; methods ; Humans ; Liquid-Liquid Extraction ; Proteins ; isolation & purification ; Solid Phase Extraction