The study investigated the intrinsic changes in material basis of Angelicae Sinensis Radix during wine processing by headspace-gas chromatography-ion mobility spectrometry(HS-GC-IMS), headspace-solid phase microextraction-gas chromatography-mass spectrometry(HS-SPME-GC-MS), and ultra-high performance liquid chromatography-quadrupole-orbitrap mass spectrometry(UPLC-Q-Orbitrap-MS) combined with chemometrics. HS-GC-IMS fingerprints of Angelicae Sinensis Radix before and after wine processing were established to analyze the variation trends of volatile components and characterize volatile small-molecule substances before and after processing. Principal component analysis(PCA) and orthogonal partial least squares-discriminant analysis(OPLS-DA) were employed for differentiation and difference analysis. A total of 89 volatile components in Angelicae Sinensis Radix were identified by HS-GC-IMS, including 14 unsaturated hydrocarbons, 16 aldehydes, 13 ketones, 9 alcohols, 16 esters, 6 organic acids, and 15 other compounds. HS-SPME-GC-MS detected 118 volatile components, comprising 42 unsaturated hydrocarbons, 11 aromatic compounds, 30 alcohols, 8 alkanes, 6 organic acids, 4 ketones, 7 aldehydes, 5 esters, and 5 other volatile compounds. UPLC-Q-Orbitrap-MS identified 76 non-volatile compounds. PCA revealed distinct clusters of raw and wine-processed Angelicae Sinensis Radix samples across the three detection methods. Both PCA and OPLS-DA effectively discriminated between the two groups, and 145 compounds(VIP>1) were identified as critical markers for evaluating processing quality, including 4-methyl-3-penten-2-one, ethyl 2-methylpentanoate, and 2,4-dimethyl-1,3-dioxolane detected by HS-GC-IMS, angelic acid, β-pinene, and germacrene B detected by HS-SPME-GC-MS, and L-tryptophan, licoricone, and angenomalin detected by UPLC-Q-Orbitrap-MS. In conclusion, the integration of the three detection methods with chemometrics elucidates the differences in the chemical material basis between raw and wine-processed Angelicae Sinensis Radix, providing a scientific foundation for understanding the processing mechanisms and clinical applications of wine-processed Angelicae Sinensis Radix.
Wine/analysis* ; Gas Chromatography-Mass Spectrometry/methods* ; Chromatography, High Pressure Liquid/methods* ; Angelica sinensis/chemistry* ; Solid Phase Microextraction/methods* ; Drugs, Chinese Herbal/isolation & purification* ; Chemometrics ; Volatile Organic Compounds/chemistry* ; Principal Component Analysis ; Ion Mobility Spectrometry/methods*

Galli Gigerii Endothelium Corneum(GGEC) is commonly used for the clinical treatment of indigestion, vomiting, diarrhea, and infantile malnutrition with accumulation. In recent decades, omnivorous domestic chickens, the original source of GGEC, has been replaced by broilers, which may lead to significant changes in the quality of the yielding GGEC. Through subjective and objective sensory evaluation, biological evaluation, and chemical analysis, this study compared the odor and quality between GGEC derived from domestic chickens and that from broilers. The odor intensity between them was compared by odor profile analysis and it was found that the fishy odor of GGEC derived from domestic chickens was significantly weaker than that of GGEC from broilers. Headspace-solid phase microextraction-gas chromatography-triple quadrupole tandem mass spectrometry(HS-SPME/GC-QQQ-MS/MS) suggested that the overall odor-causing chemicals were consistent with the fishy odor-causing chemicals. According to the odor activity va-lue and the orthogonal partial least squares discriminant analysis(OPLS-DA) result, dimethyl trisulfide, 2-methoxy-3-isobutylpyrazine, and 2-methylisoborneol were responsible for the fishy odor(OAV≥1) and the content of fishy odor-causing chemicals in GGEC derived from broilers was 1.12-2.13 folds that in GGEC from domestic chickens. The average pepsin potency in GGEC derived from broilers was 15.679 U·mg~(-1), and the corresponding figure for the medicinal from domestic chickens was 26.529 U·mg~(-1). The results of pre-column derivatization reverse-phase high-performance liquid chromatography(RP-HPLC) assay showed that the content of total amino acids and digestion-promoting amino acids in domestic chickens-derived GGEC was 1.12 times and 1.15 times that in GGEC from broilers, and the bitter amino acid content was 1.21 times folds that of the latter. In conclusion, GGEC derived from domestic chickens had weaker fishy odor, stronger enzyme activity, higher content of digestion-promoting amino acids, and stronger bitter taste than GGEC from broilers. This study lays a scientific basis for studying the quality variation of GGEC and provides a method for identifying high-quality GGEC. Therefore, it is of great significance for the development and cultivation of GGEC as both food and medicine and breeding of corresponding varieties.
Animals ; Odorants/analysis* ; Chickens ; Gas Chromatography-Mass Spectrometry/methods* ; Tandem Mass Spectrometry ; Solid Phase Microextraction ; Amino Acids ; Endothelium/chemistry* ; Volatile Organic Compounds/analysis*

OBJECTIVES: To explore the relationship between the change rules of volatile organic compounds （VOCs） in rat muscle and postmortem interval （PMI）. METHODS: A total of 120 healthy rats were divided randomly into 12 groups （10 for each group）. After the rats were sacrificed by cervical dislocation, the bodies were kept at （25±1） ℃. Rat muscle samples were separately obtained at 12 PMI points, including 0, 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9 and 10 d. The VOCs in rat muscles were collected, detected and analyzed by headspace solid-phase microextraction （HS-SPME） coupled to gas chromatography-mass spectrometer （GC-MS）. RESULTS: In total, 15 species of VOCs were identified, including 9 aromatic compounds, 3 sulfur compounds, 2 aliphatic acids and 1 heterocyclic compound. The species of VOCs increased with PMI： no species were detected within 1 day, 3 species were detected on day 2, 9 on day 3, 11 on day 4, 14 from day 5 to 7, and 15 from day 8 to 10. Total peak area of 15 species of VOCs was significantly correlated to PMI （adjusted R²=0.15-0.96）： the regression function was y=-17.05 x²+ 164.36 x-246.36 （adjusted R²=0.96） from day 2 to 5, and y=2.24 x+101.13 （adjusted R²=0.97） from day 6 to 10. CONCLUSIONS The change rules of VOCs in rat muscle are helpful for PMI estimation.
Animals ; Autopsy ; Gas Chromatography-Mass Spectrometry/methods* ; Muscles/pathology* ; Rats ; Solid Phase Microextraction ; Volatile Organic Compounds/chemistry*

OBJECTIVEHeadspace solid-phase microextraction (HS-SPME) was used pre-concentration procedure for the determination of tetrahydrofuran in urine by gas chromatography with hydrogen flame detector.

METHODSSeveral parameters controlling SPME was studied and optimised: SPME fiber, extraction time and extraction temperature, desorption time and desorption temperature.

RESULTSUnder optimal conditions, the correlation coefficient was 0.9998 and good recoveries (range from 93.0% ∼ 100.8%) were achieved, the detection limit was 0.5 µg/L.

CONCLUSIONThe method can be applied to the determination of trace amount of tetrahydrofuran in urine.

Chromatography, Gas ; methods ; Furans ; urine ; Humans ; Occupational Exposure ; analysis ; Solid Phase Microextraction ; methods

OBJECTIVETo analyze components of volatile oil from the herb of Pimpinella candolleana.

METHODThe components of volatile oil were investigated by SPME-GC-MS.

RESULTSixty-five compounds were identified which accounted for 92. 17% of total volatile oil.

CONCLUSIONThe main constituents in the essential oil were alpha-zingiberene (24.82%), pregeijerene (16.27%), beta-bisabolene (4. 82%), 2-isopropyl-5-methyl-9-methylene-bicyclo [ 4. 4. 0] dec-l-ene (4.03%), beta-sesquiphellandrene (3.98%), trans-beta-farnesene (3.68%), ar-curcumene (3.54%).

Gas Chromatography-Mass Spectrometry ; methods ; Hydrocarbons, Cyclic ; analysis ; Oils, Volatile ; chemistry ; isolation & purification ; Pimpinella ; chemistry ; Plant Oils ; chemistry ; isolation & purification ; Plants, Medicinal ; chemistry ; Sesquiterpenes ; analysis ; Solid Phase Microextraction ; methods

The current methods to prepare and determine pesticide residues in Chinese herbal medicine were summarized in this paper. In addition,the new techniques to prepare and determine pesticide residues used in recent years was reviewed, which included solid-phase micro-extraction (SPME) , supercritical fluid extraction ( SFE) , accelerated solvent extraction (ASE) , immune affinity chromatography (IAC), supercritical fluid chromatography (SFC), column switching high performance liquid chromatography (CSHPLC), high performance liquid chromatography/mass spectrometry (HPLC/MS), capillary electrophoresis (CE) and capillary zone electrophoresis (CZE) , and immune analysis (IA), etc. To sum up, these would bring a great progress in analysis of the pesticide residues in Chinese herbal medicine, and make it more rapidly, accurately and normatively.
Chromatography, High Pressure Liquid ; Chromatography, Supercritical Fluid ; Drugs, Chinese Herbal ; chemistry ; Electrophoresis, Capillary ; Gas Chromatography-Mass Spectrometry ; Pesticide Residues ; analysis ; isolation & purification ; Plants, Medicinal ; chemistry ; Reproducibility of Results ; Solid Phase Microextraction ; Technology, Pharmaceutical ; methods