Association between single nucleotide polymorphism in exon 33 of thyro-globulin gene and Graves ’ disease relapse after antithyroid drug with-drawal / 中国病理生理杂志

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.

Metabonomic study on protective effect of ethanol extracts of drynariae rhizoma on osteoporosis in rats urine by using UPLC-MS/MS / 中国中药杂志

This paper was designed to study metabonomic characters of the osteoporosis induced by high dose of hydrocortisone and the protective effects of Drynariae Rhizoma, which can replenish the kidney and strengthen the bones. A urinary metabonomics method based on ultra-performance liquid chromatography coupled with mass spectrometry (UPLC-MS/MS) was developed. Clear separation of healthy control group, model group and treatment group was achieved by using the principal components analysis (PCA) and 9 significantly changed metabolites were identified as potential biomarkers of osteoporosis. Compared with the health control group, the model group rats showed lower levels of creatinine, citric acid, azelaic acid, hippurate, tryptophan and indoxyl sulfate together with higher levels of phenylalanine, cresol sulfate and phenaceturic acid. These changes in urinary metabolites suggest that the disorders of amino acid metabolism, energy metabolism, gut microflora and anti-oxidative damage are related to osteoporosis induced by high dose of hydrocortisone and the potential effect of Drynariae Rhizoma on all the four metabolic pathways.

Study on in vitro and in vivo material base of Sini San by UPLC-PDA-MS/MS / 中国中药杂志

<p><b>OBJECTIVE</b>To analyze chemical constituents of Sini San its migrating components in rat plasma and study its in vitro and in vivo material base using ultra-performance liquid chromatography coupled with photo-diode-array detector and tandem mass spetrometry (UPLC-PDA-MS/MS).</p><p><b>METHOD</b>ACQUITY UPLC BEH C18 column (2.1 mm x 100 mm, 1.7 microm) was adopted, with gradient elution system of water containing 2 mmol x L(-1) ammonium acetate and acetonitrile at flow rate of 0.2 mL x min(-1). The column temperature was maintained at 35 degrees C. The mass spectra were obtained by electrospray ionization source operating in both positive and negative ion mode. Ions were scanned from the m/z 100 to 1 000, and the characteristic ions were schizolysised twice to obtain the secondary MS data.</p><p><b>RESULT</b>Twenty chemical constituents were detected, including paeoniflorin, glycyrrhizic acid, saikosaponins a and naringin. In vivo, there were 8 ingredients directly absorbed into blood after the administration of Sini San decoction, such as paeoniflorin, naringin and hesperidin. Besides, 6 metabolites were also detected, involving glucuronides, sulfate and sulfoglucuronides.</p><p><b>CONCLUSION</b>In vitro and in vivo chemical materials of Sini San decoction is analyzed by UPLC-PDA-MS/MS to reflect in vitro and in vivo material base of Sini San decoction in a comprehensive and rapid manner and provide basis for further study on efficacious material basis of Sini San decoction.</p>

LC-MS/MS method for quantification and pharmacokinetic study of gabapentin in human plasma / 药学学报

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.

Simultaneous assay of epimedin A epimedin B, epimedin C and icariin in herba epimedii by QAMS / 中国中药杂志

<p><b>OBJECTIVE</b>To establish a new method and validate its feasibilities for quality evaluation of Fructus Epimedii.</p><p><b>METHOD</b>Four 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.</p><p><b>RESULT</b>No significant differences were found in the quantitative results of three flavones by external standard method and QAMS method.</p><p><b>CONCLUSION</b>It is feasible and accurate to evaluate the quality of Fructus Epimedii.</p>

Isolation and identification of chemical constituents of fruits of Acanthopanax sessiliflorus / 中国中药杂志

<p><b>OBJECTIVE</b>To isolate and elucidate the chemical constituents of the fruits of Acanthopanax sessiliflorus.</p><p><b>METHOD</b>Isolation and purification were carried out on the column chromatography of silica gel and Sephadex LH-20. Their structures were elucidated on basis of physicochemical properties and spectral data.</p><p><b>RESULT</b>Nine compounds were isolated and identified as oleanolic acid-3-O-6'-O-methyl-beta-D-glucuronopyranoside (1), 22-alpha-hydroxychiisanogenin (2), oleanolic acid-3-O-beta-D-glucuronopyranoside (3), oleanolic acid-3-O-beta-D-glucopyranoside (4), oleanolic acid (5), chiisanogenin (6), (-)-sesamin (7), daucosterol (8), beta-sitosterol (9).</p><p><b>CONCLUSION</b>Compound 1 is obtained from the genus Acanthopanax genus for the first time. Compounds 2-5 are isolated from this plant for the first time.</p>

Quality Standard of Desheng Pills / 中国药房

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.

HPCE DETERMINATION OF TRIMEBUTINE MALEATE IN RAT PLASMA AND ITS PHARMACOKINETICS / 药学学报

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.

Study on the Preparation Technique and Quality of Xuelian Freeze-dry Sterile Injection powder / 中国药房

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.

Pharmacological effects of Gushudan against osteoporosis / 中草药

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.

Fingerprints of Xinshu Oral Liquid by HPCE / 中草药

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.

Determination of prim-O-glucosylcimifugin and 4′-O-?-D-glucosyl-5-O-methylvisamminol in Ganmaoqingre Granules by RP-HPLC / 中成药

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.