High-performance countercurrent chromatography (HPCCC) coupled with reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed to isolate dihydrophaseic acid 3′-O-β-D-glucopyranoside (DHPAG) from the extract of Nelumbo nucifera seeds. Enriched DHPAG sample (2.3 g) was separated by HPCCC using ethyl acetate/n-butanol/water system (6:4:10, v/v/v, normal-phase mode, flow rate: 4.0 mL/min) to give 23.1 mg of DHPAG with purity of 88.7%. Further preparative RP-HPLC experiment gave pure DHPAG (16.3 mg, purity > 98%). The current study demonstrates that utilization of CCC method maximizes the isolation efficiency compared with that of solid-based conventional column chromatography.
Chromatography ; Chromatography, Liquid ; Countercurrent Distribution ; Methods ; Nelumbo

Chromatography, Gas ; methods ; Triazoles ; blood

Biocompatible Materials ; analysis ; Chromatography ; methods ; Chromatography, Gas ; methods ; Chromatography, Liquid ; methods ; Paraquat ; analysis ; Pesticide Residues ; analysis

Metabonomics involves the unbiased quantitative and qualitative analysis of the complete set of metabolites present in cells, body fluids and tissues (the metabolome) based on modern analytic technique with high throughput, high sensitivity, and high resolution. Gas chromatography-mass spectrometry (GC-MS) is used to gain qualitative results of detected metabolites for biological samples as it provides superior distinguishability, detection sensitivity and integrated standard mass spectrometry library. In this article, the historic developments of GC-MS and its application in metabonomics in the past several years were reviewed. Firstly, the classification and the derivative methods of GC-MS were introduced. Subsequently, sample pretreatment process, qualitative and quantitative analysis and data analysis during detecting metabolites by GC-MS were introduced, then its application in microorganism, plant and disease diagnosis was systematically summarized. Finally, the problems in metabonomics study based on GC-MS and the research prospect in the future were discussed.
Gas Chromatography-Mass Spectrometry ; methods ; Metabolomics ; methods

OBJECTIVETo establish a method for simultaneous determination of 17 common pesticides in whole blood by solid phase extraction-gas chromatography-mass spectrometry (SPE-GC-MS).

METHODSWhole blood samples were treated by extraction with acetonitrile, and the obtained extract was cleaned up using an Oasis HLB SPE cartridge; pesticides were separated by GC and quantitatively analyzed by MS with selected ion monitoring.

RESULTSThe concentrations of 17 pesticides in whole blood were 1.0-5.0 mg/L, and the recovery rate was 41.3-102.1%, with a relative standard deviation of less than 10%in most pesticides. The 17 pesticides showed a good linear relationship between concentration and peak area within 0.5-5.0 mg/L, with a correlation coefficient of 0.9945-0.9994. The limit of detection and limit of quantification were 0.02-0.05 mg/L and 0.05-0.09 mg/L, respectively.

CONCLUSIONWith this method, 17 pesticides in whole blood can be well separated and determined. This method has high sensitivity, accuracy, and precision and can be used for identification and quantification of multiple pesticides in blood samples.

Objective: To establish a method for the rapid determination of acetaminophen (APAP) in human plasma by LC-MS/MS. Methods: The plasma samples were extracted by methanol and acetonitrile (1: 1) and purified directly. C(18) column was used for sample separation. The mobile phase were methanol (5 mmol/L ammonium acetate) and water (5 mmol/L ammonium acetate). Samples were analyzed by LC MS/MS with the electrospray ionization multi reaction monitoring (MRM) mode. Results: The calibration curves of APAP was linear in the concentration range of 0~10 mg/L, the correlation coefficient (r) was greater than 0.999 0. The relative standard deviation within and between batches was less than 10%. The recovery rate were 96.81%~101.7%. The detection limit of the method was 0.1 μg/L and the lower limit of quantification was 0.3 μg/L. Conclusion: This method has strong specificity, high sensitivity and reliable determination results. It is suitable for the rapid analysis of clinical plasma samples.
Humans ; Chromatography, Liquid/methods* ; Acetaminophen ; Tandem Mass Spectrometry/methods* ; Methanol ; Chromatography, High Pressure Liquid/methods*

OBJECTIVES: To establish a simple and rapid qualitative and quantitative detection method of dexmedetomidine in blood. METHODS: Blood was separated on the Allure PFP Propyl liquid chromatography column with isocratic elution after it was precipitated by acetonitrile and filtered. Qualitative and quantitative analysis of dexmedetomidine was performed using positive ion scan mode and multi-reaction monitoring mode. RESULTS: The limit of detection of dexmedetomidine in blood was 0.2 ng/mL and the limit of quantification was 0.5 ng/mL. The linearity of the method was good in the range of 0.5-1 000 ng/mL, and the correlation coefficient was greater than 0.99. The accuracy of the method was 90.34%-112.67% and the extraction recovery was 50.05%-91.08%, with no significant matrix effect. CONCLUSIONS This method is simple, selective and suitable for the qualitative and quantitative analysis of dexmedetomidine in blood, which can provide a reference for drug-facilitated cases involving dexmedetomidine.
Tandem Mass Spectrometry/methods* ; Chromatography, High Pressure Liquid/methods* ; Dexmedetomidine/analysis* ; Reproducibility of Results ; Chromatography, Liquid/methods*

OBJECTIVETo evaluate the quality of Polygonum perfoliatum collected from GAP planting base efficiently so as to provide scientific evidence for its GAP tending plant by HPLC fingerprinting method.

METHODAnalysis was performed on a reserved-phase column Lichrosher-C18 column (4.6 mm x 250 mm, 5 microm), A linear gradient elution of 0.2% aqueous acetic acid and acetonitrile was used for the separation.

RESULTWildlife tending P. perfoliatum was relatively stable. The chromatograms of the samples from 2011 were more accordant than those from 2010. Samples in Dafang were the most stable and had little differences during the two years. The quality of P. perfoliatum planted in the regions of sample GBG-(GD) 002 in Guiding and sample GBG-(LL) 003 in Longli were more stable and better than those from other regions.

CONCLUSIONIt is a feasible method that can be used to evaluate the quality of P. perfoliatum for GAP planting.

OBJECTIVETo develop a method for determining the concentration of dichlorvos in serum by gas chromatography and to provide a basis for clinical diagnosis and monitoring of dichlorvos poisoning.

METHODSThe serum (0.5 ml)collected from patients with dichlorvos poisoning was mixed with ethyl acetate (2.0 ml) and underwent shaking/extraction; the obtained liquid was subjected to standing (5 min) and centrifuging (4000 rpm); the obtained supernatant was collected and blow-dried with nitrogen and was then dissolved in ethanol (50 µl); 1.0 µl of the obtained liquid was collected and loaded into a glass-packed column; gas chromatography was performed using a nitrogen-phosphorus detector.

RESULTSA linear relationship was found when the concentration of dichlorvos in serum was 5.0 ∼ 50.0 µg/ml, with a regression equation of y = 804.13x-691.8 (r = 0.9992). The minimum detectable concentration was 2.0 µg/ml, the recovery rate was 86.8% ∼ 94.5%, the relative standard deviation (RSD) was 4.6% ∼ 5.5%, with an intra-day RSD of 4.52% ∼ 5.21% and an inter-day RSD of 3.56% ∼ 5.52%.

CONCLUSIONThis determination method is easy to operate, efficient, and accurate, and can be used for quickly diagnosing dichlorvos poisoning and quantitatively evaluating treatment outcome.

Chromatography, Gas ; methods ; Humans ; Tetrachloroethylene ; blood