AIM　To develop a method for the determination of trimebutine maleate in rat plasma by using high performance capillary electrophoresis. The method was employed to pharmacokinetic analysis of trimebutine maleate. METHODS　Plasma samples were deproteinized with acetonitrile (containing ephedrine hydrochloride as internal standard) and the supernatant was dried under N2 stream at 50℃. The residue was dissolved with methanol-water (1∶1) and injected into the capillary by siphon. The electrophoresis was performed in uncoated fused-silica capillary and the voltage was 10 kV. The running buffer was 0.03 mol*L-1 NaH2PO4 (pH 6.0). The eluate was detected at 214 nm by UV detection. RESULTS　The recovery for trimebutine maleate in rat plasma was 72.8%-87.9%. The calibration curve in plasma was linear over the range 5-200 μg*L-1. The limit of quantitation was 5 μg*L-1. The intraday relative standard deviation (n=6) and the interday relative standard deviation (n=18) were less than 14%. The highest concentration in plasma was observed at 30 min after ig trimebutine maleate to rats. The pharmacokinetic results were AUC0-∞=8 μg*min*mL-1, T1/2(Ke)=173 min and Ke=5.6×10-3 min-1. CONCLUSION　The method is accurate, sensitive and suitable for pharmacokinetic study of trimebutine maleate.

Objective: A reversed phase HPLC method was described for determination of prim O glucosylcimifugin and 4′ O ? D glucosyl 5 O methylvisamminol in Ganmaoqingre Granules. Methods:The sample was separated on ODS column with mobile phase of methanol 40 mmol?L -1 sodium acetate pH 6.9 (35∶65) for prim O glucosylcimifugin and H 2O methanol THF(62∶38∶1) for 4′ O ? glucosyl 5 O methylvisamminol. The flow rate was 0.8 mL?min -1 , and the detection was set at 254 nm. Results: The calibration curves were linear in the range of 0.72 ?g?mL -1 ～6.5?g?mL -1 for prim O glucosylcimifugin and 0.92?g?mL -1 ～16.5?g?mL -1 for 4′ O ? D glucosyl 5 O methylvisamminol( r =0.9999). The average recovery was 100.3% and 94.7%. The content of prim O glucosylcimifugin and 4′ O ? D glucosyl 5 O methylvisamminol in Ganmaoqingre Granules was 0.133 mg?g -1 and 0.167 mg?g -1 , respectively. Conclusion: The method is fast and specific for both constitutents of Ganmaoqingre Granules.

A sensitive, rapid and specific liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for quantification of gabapentin in human plasma has been developed. After a single plasma protein precipitation with methanol, gabapentin and metformin (internal standard) were chromatographed on a Inertsil ODS-3 column (50 mm x 2.1 mm ID, 3 microm) with mobile phase consisting of methanol-0.2% formic acid aqueous solution (80:20, v/v) at a flow-rate of 0.2 mL x min(-1). Electrospray ionization (ESI) source was applied and operated in the positive ion mode. Multiple reaction monitoring (MRM) mode with the transitions of m/z 172 --> m/z 154 and m/z 130 --> m/z 71 were used to quantify gabapentin and metformin, respectively. The run time was 2.2 min. The linear calibration curve was obtained in the concentration range of 40.8-8.16x10(3) ng x mL(-1). The lower limit of quantification was 40.8 ng x mL(-1). The intra- and inter-day precision (RSD) was less than 12%, and the accuracy (RE) was within +/-6.4% calculated from quality control (QC) samples. The method was used to determine the concentration of gabapentin in human plasma after a single oral administration of 600 mg gabapentin capsule to 20 healthy male Chinese volunteers. The method was proved to be selective, sensitive, rapid and suitable for pharmacokinetic study of gabapentin in human plasma.

Objective To develop a method of quality control for fingerprints of Xinshu Oral Liquid. Methods Based on electrophoregram of ten batches of genuine Radix Angelicae Sinensis (RAS), ten batches of genuine Rhizoma Chuanxiong (RC), and ten batches of genuine Flos Carthami (FC) by high performance capillary electrophoresis (HPCE) to compare the fingerprints between Xinshu Oral Liquid and the genuine medicinal herbs, single herb decoction, nagetive control herb solution, respectively. The fingerprint assignment was made by comparing the UV spectra and relative migration time. Results To compare the fingerprints of ten samples from different batches and single herb, the correlation of peaks between fingerprings was found. Finally the standard fingerprints and the method of quality control were established. Conclusion Based on the fingerprints of ten batches of prearations, an average electro-phoregram was used as the standard fingerprint. There are 27 “common peaks” in the fingerprint, among them 14 from RAS, ten from RC (in which seven are commnon) and nine from FC.

Objective To investigate the preventive effects of Gushudan on osteoporosis in rats after administrated prednisolone.Methods Wistar male rats(60) were divided into six groups: control group,model group,Gushudan groups(3,1,and 0.3 g/kg),and Gushukang 1 g/kg group.The effect was observed by measuring the levels of blood calcium,blood phosphorus,blood BGP content,bone calcium,bone phosphorus,bone density,and hone biomechanics.Results After eight weeks,Gushudan significantly increased the bone density,bone biomechanics,blood BGP content,bone calcium,and bone phosphorus in model group rats.Conclusion Gushudan could increase bone density,bone biomechanics,blood BGP content,bone calcium,and bone phosphorus induced by prednisolone.These results suggest that Gushudan has a distinct preventive effect on osteoporosis rats.

OBJECTIVE:To prepare xuelian freeze-dry sterile injection powder and to establish a quality control for this drug.METHODS:The best formulation and preparation technique of the powder for injection was optimized by screening the variety and quantity of vehicle;the contents,which were determined by UV,together with the finger print were taken as the main index to study the quality.The stability was observed through long test.RESULTS:Take the40%mannitol as excipient;The mean recovery results was99.4%(RSD=0.90%);The freeze-dry sterile injection powder could be reflection the finger print character of extract fluid better than injection.The preparation was stable after12months storage at room tempera-ture.CONCLUSION:The formulation is reasonable,the preparation technique is feasible and the quality is controllable.

OBJECTIVE:To establish the quality standard of Desheng pills. METHODS:The components Leonurus japonicus,Bupleurum chinense and Aucklandia lappa in Desheng pills were qualitatively identified by TLC,and the content of peoniflorin in Desheng pills was determined by HPLC. RESULTS:The TLC spots of L. japonicus,B. chinense and A. lappa were clear. The linear range of peoniflorin was 1.40～28.0 ?g?mL-1(r=0.999 0) with an average recovery of 99.4%(RSD=1.5%,n=9). CONCLUSION:The established standard can be used for the quality control of Desheng pills.

OBJECTIVETo establish a new method and validate its feasibilities for quality evaluation of Fructus Epimedii.

METHODFour main effective flavones, epimedin A, epimedin B, epimedin C and icariin were selected as analytes to evaluate the quality of Fructus Epimedii. The relative correction factors (RCF) of icariin to the other three flavones were calculated. The method was evaluated by comparison of the quantitative results between external standard method and QAMS method.

RESULTNo significant differences were found in the quantitative results of three flavones by external standard method and QAMS method.

CONCLUSIONIt is feasible and accurate to evaluate the quality of Fructus Epimedii.

Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; chemistry ; Flavonoids ; analysis ; Reproducibility of Results ; Statistics as Topic ; methods ; Time Factors

AIM:To explore the association between single nucleotide polymorphism in exon 33 (E33SNP) of thyroglobulin gene and Graves ’ disease ( GD) relapse after antithyroid drug ( ATD) withdrawal .METHODS:The healthy controls (232 cases) and GD patients with discontinued treatment (243 cases) were selected.According to the time of re-lapse, the GD patients were divided into A, B and C subgroups.The A group contained 77 cases of relapse within 1 year, B group contained 86 cases of relapse 1~2 years after treatment and C group contained 80 cases without recurrence within 2 years.The genotypes of E33SNP were identified by RT-PCR.The genotype ratio of thyroglobulin between control group and observation group was comparatively analyzed , and the levels of thyroid-stimulating hormone ( TSH) , free triiodothyro-nine (FT3), free thyroxine (FT4) and thyrotropin receptor antibody (TRAb), ophthalmopathy and goiter size in A , B and C subgroups in different genotype GD patients were investigated .Moreover , cumulative efficiency for patients with different genotypes in the observation group after ATD treatment within 2 years were analyzed .RESULTS:The genotype of E33SNP between observation group and control group had no significant difference , but a significant difference between A , B and C subgroups was observed (P<0.05).The levels of TSH, FT3 and FT4, and goiter size of the patients with different geno-types had no significant difference , while the TRAb levels and ophthalmopathy presented a significant difference ( P <0.05).In addition, the cumulative efficiency within 2 years for GD patients with E33SNP T/T, E33SNP T/C and E33SNP C/C genotypes was 61.8%, 42.6% and 21.3%, respectively, all with significant differences (P<0.05).CONCLU-SION:The GD patients with E33SNP C/C genotype have significantly higher TRAb level and ophthalmopathy rate than those in the patients with E33SNP C/T and E33SNP C/C genotypes, and are more likely to relapse after ATD treatment . The GD patients with E33SNP T/T genotype show a lower recurrence rate .Therefore, combination treatment or other treat-ment modalities may be more reasonable for the GD patients with E 33SNP C/C genotype.

Objective To understand the prevalence of metabolic syndrome in Gansu.Methods A multistage stratified cluster sampling method was conducted.A total of 6 609 adults (range 18-96 years old) from 5 cities located in different areas of Gansu province were included in the analyses and all of them underwent physical examinations.Metabolic syndrome was diagnosed under the modified 2005 National Cholesterol Education Program Adult Treatment Panel Ⅲ (ATP Ⅲ) guidelines as well as the 2004 Chinese Diabetes Society (CDS) guidelines.Results Using the modified ATP Ⅲ criterion for diagnosis,the unadjusted prevalence rate of metabolic syndrome was 30.43％ (35.25％ in males and 23.02％ in females,respectively) and the age-adjusted prevalence was 29.05％.The prevalence of metabolic syndrome increased with age.Combination of central obesity,high TG hyperlipidemia and low HDL-C hyperlipidemia was most frequently seen.Under the CDS criterion,the unadjusted prevalence of metabolic syndrome was 13.42％,with the age-adjusted prevalence as 12.65％.A low level of agreement between the ATP Ⅲ and CDS was observed (Kappa index=0.496).Conclusion Under the ATP Ⅲ definition,more adults with MS were identified thus could be recommended as the preferred diagnostic criterion.Metabolic syndrome had become a noteworthy public health problem.Prevention programs related to metabolic syndrome should be urgently warranted.