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 investigate the effect of different chromatographic conditions on QAMS relative correlation factors (RCF) and relative retention values (RT(R)).

METHODC18 columns were used with methyl alcohol-0.4% phosphoric acid water (85: 15) as the mobile phase. The detection wavelength was 254 nm, the column temperature was 30 degrees C, and the flow rate was 1.0 mL x min(-1). The five anthraquinones in Rhei Radix et Rhizoma were selected to be the objects of study. The RCF and RT(R) among aloe-emodin, rhein, chrysophanol, physcion and emodin were determined under different chromatographic conditions.

RESULTTheir RCFs showed no significant difference.

CONCLUSIONThe RCFs among anthraquinones established by QAMS can be used as a constant in content determination of traditional Chinese medicines/patent traditional Chinese medicines.

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 develop a novel method to determine fastly and nondestructively the content of paeoniflorin, albiflorin and moisture in Radix Paeoniae Alba with near infrared diffuse reflection spectroscopy.

METHODMultivariate calibration models based on PLS algorithm were developed to correlate the spectra and the corresponding values determined by the reference method.

RESULTThe corelation coefficients (R2) of the calibration models were 0.938, 0.943 and 0.976, and the prediction average relative deviation for paeoniflorin, albiflorin and moisture content were 6.5%, 0.23% and 3.8%, respectively.

CONCLUSIONThe NIRS determination method is rapid, accurate, nondestructive and non-pollution. It can dispose the samples without complicated pretreatment. It is qualified to analyze rapidly traditional Chinese medicine whose components are complex. NIRS can be used to control the quality of herbal material of paeony formula granule.

4-Hydroxycoumarins ; blood ; Animals ; Chromatography, High Pressure Liquid ; methods

Chromatography, High Pressure Liquid ; methods ; Electrochemistry ; Homocysteine ; blood ; Humans

The concentration of 5 nucleosides, uracil, uridine, guanidine, adenine and adenosine in culture of Paecilomyces hepialid was determined by the developed method of HPLC. The HPLC method was performed on a Waters SunFire C18 (4.6 mm x 250 mm, 5 μm) column with methanol-water gradient elution as the mobile phase. The detection wavelength was 260 nm and the colunmn temperature was controlled at 30 °C. The linear range was 10.00-200.00 mg · L(-1) (r = 0.9994) for uracil, 10.10-202.00 mg · L(-1) (r = 0.9992) for uridine, 10.00-200.00 mg · L(-1) (r = 0.9991) for guanidine, 10.30-206.00 mg · L(-1) (r = 0.9992) for adenine and 10.45-209.00 mg · L(-1) (r = 0.9991) for adenosine, respectively. The RSD of precision was 0.032%, 0.035%, 0.039%, 0.049%, 0.00080%, respectively. The average recoveries of uracil, guanidine, adenine, and adenosine were 97.34%, 99.10%, 101.6%, 98.61% and 100.2% with RSD of 1.3%, 2.1%, 0.96%, 0.95%, and 1.3% respectively. The method showed high sensitivity, good selectivity, linearity and repeatability, which was suitable for the content analysis of 5 nucleosides components in P. hepialid and its extracts.
Chromatography, High Pressure Liquid ; methods ; Nucleosides ; analysis ; Paecilomyces ; chemistry

OBJECTIVETo establish a chromatographic fingerprint of Lonicera japonica and apply it to identify geo-authentic of L. japonica.

METHODThe HPLC was applied in chromatographic separation and data were analysed by "computed aided similarity evaluation" software.

RESULTThere exited distinct difference of chemical components group between and non-authentic samples.

CONCLUSIONThe established HPLC fingerprint can be used for the identification of geo-authentic of L. japonica.

This study established an HPLC fingerprint of Tibetan medicine Shaji Gao from different habitats and lay a foundation for Shaji Gao varieties identification and preparation process. The chromatographic condition was as follow: Agilent zorbax SB-C18 (4.6 mm x 250 mm, 5 μm) eluted with the mobile phases of acetonitrile and 0.4% phosphoric acid water in gradient mode. The flow rate was 1.0 mL x min(-1), and the detection wavelength was set at 360 nm. The fingerprints of 15 batches Shaji Gao were carried out by similarity comparation, 7 chromatographic peaks were extracted as the common peaks of fingerprint, 3 peaks were identified, which were quercetin, kaempferol and isorhamnetin. The similarity degrees of 14 batches of samples were above 0.9 and 1 batch of samples was below 0.9. This is the first established fingerprint of Shaji Gao by using HPLC. This method has good precision, stability and repeatability that it could provide basis for quality control and evaluation of Shaji Gao.
Chromatography, High Pressure Liquid ; methods ; Medicine, Tibetan Traditional ; Quality Control