OBJECTIVE:To establish an HPLC method for the determination of gastrodin in Choudongning capsule. METHODS:The sample was determined on Elite C18 column(250 mm?4.6 mm,5 ?m);the mobile phase consisted of methanol -water(3∶97) at a flow rate of 1.0 mL?min-1;the detection wavelength was set at 221 nm. RESULTS:The linear range of gastrodin was from 0.051 ?g to 0.357 ?g(r=0.999 9) and its average recovery was 98.99%(RSD=1.91%,n=6).CONCL-USION:The method is convenient,accurate and reproducible,and it is applicable for the quality control of Choudongning capsule.

OBJECTIVE:To establish an HPLC method for the determination of the contents of cinobufagin and resibufogenin in Yigankang capsule.METHODS:The samples were separated on Spherigel ODS C18(150 mm?4.6 mm,5 ?m)chromatographic column with 0.5% KH2PO4-acetonitrile(50∶50,pH was adjusted to 3.2 by phosphoric acid)used as a mobile phase at a flow rate of 1.0 mL?min-1.The detection wavelength was set at 296 nm and the column temperature was kept at 40 ℃.RESULTS:The linear ranges of cinobufagin and resibufogenin were 0.22～1.09 ?g(r=0.999 8)and 0.26～1.30 ?g(r=0.999 9),respectively,and the average recoveries of cinobufagin and resibufogenin were 99.4%(RSD=1.9%,n=9)and 98.7%(RSD=1.4%,n=9),respectively.CONCLUSION:This method is proved to be sensitive,simple,accurate and specific,and it is applicable for the quality control of Yigankang capsule.

OBJECTIVE:To establish the quality standard of Compound niubangzi buccal tablets.METHODS:Lonicerae japonica and Paeonia suffruticosa in the formulation were identified by TLC,and the content of arctiin in the tablets was determined by HPLC.RESULTS:The TLC spots were clear,well-isolated and distinctive.The linear range of arctiin was 0.586～5.274 ?g(r=0.999 9)and its average recovery was 98.94%(RSD=1.68%,n=9).CONCLUSION:The established quality standard can be used for the quality control of Compound niubangzi buccal tablets.

Objective To optimize extraction technology of flavonesingredients from Herba Epimedii by uniform design. Methods Ultraviolet spectrophotometry was adopted to determine the content of total flavonoids. Content of epimedin A, epimedin B,epimedin C,icariin and baohuosideⅠ were determined by HPLC. U10?( 108 ) uniform design was used to conduct the multiple comprehensive evaluation of six ingredients and comprehensively analyze the influence of the concentration and amount of ethanol, extracting time on extraction of flavonesin gredients from Herba Epimedii. Results The uniform design experiment showed that 15-fold weight of 60% ethanol,extracting 2 times and each time with 165 min were the optimum extraction condition. Conclusion The method is easy and reasonable to handle,has stable and reliable results,and good repeatability and feasibility.It can be applied in industrial production.

OBJECTIVE:To optimize water extraction technology of Shenqi yiqi capsules. METHODS:The water extraction technology of Shenqi yiqi capsules was optimized by L9(34)orthogonal test with amount of water added,decoction times and decoc-tion time as factors using the extraction rate of astragaloside,calyosin-7-O-β-D-glycoside,icariin and bergenin as index,and the verification test was made. RESULTS:The best extraction technology was as follows as 8-fold water,decocting for 3 times,2 h each time;comprehensive score of 3 batches of samples in validation test were 98.95,99.71 and 99.98(RSD<2%,n=3). CON-CLUSIONS:The water extraction technology optimized by multi-index comprehensive score-orthogonal test is stable,scientific and reasonable.

Amyloidosis ; Gastrointestinal Hemorrhage ; Humans ; Immunoglobulin Light-chain Amyloidosis

The chemical components of mainstream smoke were trapped by the artifical salvia. A novel method) for the analysis of the trapped chemical components was established using stir bar sorptive extraction(SBSE)) followed by a thermal desorption-gas chromatography-mass spectrometry(TD-GC-MS). The major) factors including desorption temperature, desorption time, cryofocusing temperature, extraction time and the addition of sodium chloride were studied. Under the optimized conditions, the average relative standard deviation(RSD) of peak areas of 44 components which were identified from the artifical saliva for 6 determinations was less than 10%, which showed the good repeatability of this method. The experiment result indicated that the SBSE-TD-GC-MS technique provided a powerful tool for the analysis of smoke components of some cigarette) trapped and dissolved in the saliva.

OBJECTIVE:To optimize the extraction technology of garlic oil. METHODS:Using extraction rate of garlic oil as index,based on single factor test,Box-Behnken response surface method was used to optimize conditions of steam distillation method for the extraction of garlic as fermentation time,solid to liquid ratio,fermentation temperature and the verification test were made for the optimized technology. RESULTS:The optimal extraction technology was as follows as fermentation time of 4.5 h,solid to liquid ratio of 1:7,fermentation temperature of 55 ℃. The average extraction rate of garlic oil in verification test was 0.32%(RSD=1.43%,n=3);the relative error between the measured value and predicted value was 0.06%. CONCLUSIONS:Box-Behnken response surface method is simple,reasonable and feasible to optimize the extraction technology of garlic oil,which can provide a scientific basis for industrial production.

Objective To investigate the characteristics and significance of atypical flow cytometric immunophenotype in plasma cell myeloma.Methods Using case-control study , 48 cases with atypical immunophenotype of plasma cell myeloma and 42 cases as control group were studied by flow cytometry , the former cases were classified into three groups according to the expression of CD 38, CD138, CD19, CD56 :CD38 +/CD138 +/CD19 +/CD56 +, CD38 +/CD138 +/CD19 +/CD56 -, CD38 +/CD138 +/CD19 -/CD56 -.And compare the three groups with intracellular immunoglobulin light chain (cKappa, cLambda) , bone marrow morphology and immunofixation.The positive rate was compared with chi-square test.Results Bone marrow plasma cells showed expression of particular antigens in the following proportion of the 48 cases:CD45 29.17%, CD38 100%, CD138 100%, CD19 95.83%, CD56 43.75%, cKappa 43.75%and cLambda 56.25%.And in the three groups , the expression of monoclonal immunoglobulin were 43.75%, 52.08%and 4.17%, which bone marrow morphology and immunofixation were 57.14%,80%, 100%and 71.43%,88%,100%.The positive rate of flow cytometry , bone marrow morphology and serum immunofixation electrophoresis were 100%, 70.83% and 81.25%.While the expression of particular antigens in the control group were:CD45 47.62%, CD38 100%, CD138 100%, CD19 100%, CD56 0%, cKappa 100% and cLambda 100%.And no abnormalities were detected in bone marrow morphology and immunofixation.Conclusions Compared with the bone marrow morphology and immunofixation , multiparameter flow cytometry has more helpful to find out atypical immune phenotype of plasma cell myeloma, and differentiate malignant and benign plasma cell , contributes to the diagnosis of clinical plasma cell myeloma, prognosis and treatment monitoring.

Objective The quality evaluation of the Shuwei mixture was determined by the content of the six components of sinapine cyanide sulfonate, magnolol, honokiol, hesperidin, naringin and neohesperidin. Methods RP-HPLC method was used.The separation was performed on a Agilent ZORBAX Eclispse SB-C18column (4.6 mm×250 mm,5 mm),the mobile phase consisted of acetonitrile(A)-0.1% phosphoric acid with gradient elution at the flow rate of 1.0 mL·min-1.The detection wavelength was 326 nm ( sinapine cyanide sulfonate ), 294 nm ( magnolol, honokiol ) and 283 nm ( naringin, neohesperidin).The column temperature was kept at 30 ℃. Results The sinapine cyanide sulfonate, magnolol, honokiol, hesperidin,naringin and neohesperidin all had good linear relationship in the ranges of 0.049 6-1.24,0.048 2-1.205,0.060 5-1.512 5,0.187 2-4.68,0.131 6-3.29,0.197-4.925 μg.The average recoveries were 100.66%, 99.86%, 101.37%, 102.41%, 99.01%, 102.05%, respectively, RSD were 0.82%, 1.89%, 2.56 %, 0.74%, 1.54%, 0.99%, respectively. Conclusion The method is simple,accurate,reproducible and nice to the separation,and can be used for the quality evaluation of Shuwei mixture.