AIM: To establish the quality standard of Wumeirendan (Fructus Mume, Radix et Rhizoma Glycyrrhizae, Mentholm, etc.) METHODS: Fructus Mume was identified by TLC. Menthol was determined by GC, Ammonium glycyrrhiziate was determined by HPLC. RESULTS: The average recoveries were 103.5% and 100.3%, RSD were 0.76% and 1.03%. The TLC sports developed were fairly clear, and the blank test showed no interference. CONCLUSION:The method developed is simple and accurate with good reproducibility, and the method can be used for quality control of Wumeirendan.

AIM: To establish the quality standard of Yupingfeng Oral Liquid(Radix Astragali,Radix Sapo-shnikoviae,Rhizoma Atractylodis Macrocephalae,etc.); METHODS:Rhizoma atractylodis macrocephalae was (identified) by TLC,Radix Saposhnikoviae was identified by HPLC;astrayloside Ⅳ was determined by HPLC.( RESULTS):The recovery of astragloside Ⅳ was 96.7%,RSD was 1.74%.The TLC sports developed were fairly clear,and the blank test showed no interference. CONCLUSION:The mothod developed is simple and accurate with good reproducibility,and the mothod can be used for quality control of Yupingfeng Oral Liquid. withgood

AIM: To establish the GC method for the determination of linalool of Rhizoma Homalomenae. METHODS:The column consisted of Fused Silica Capillary Polyethylene Glyol(30 m?0.25 mm?0.25 ?m),column temperature was at 120 ℃,Injection port temperature at 260 ℃,Detector temperature at 300 ℃,flow rate was 1.0 ml/min. RESULTS: Linalool has a good linearity in the range of 0.011 985～1.997 5 ?g.The recovery rate was 99.2%,RSD was 1.63%. CONCLUSION: The method developed is simple and accurate with good reproducibility,and can be used for quality control of Rhizoma Homalomenae.

This paper aims to establish a method for the determination of sulfur dioxide in sulfur fumigation Chinese herbs. Sample powder and hydrochloric acid solution were isolated by paraffin layer in order to avoid early reactions, with the generation of sulfur dioxide, headspace with airtight needle was used to transfer sulfur dioxide into gas chromatograph, and detected with thermal conductivity detector. The analytical performance was demonstrated by the analysis of 12 herbs, spiked at four concentration levels. In general, the recoveries ranging from 70% to 110%, with relative standard deviations (RSDs) within 15%, were obtained. The limit of detection (LOD) was below 10 mg x kg(-1). Standard addition can be used for low recovery samples. The method is simple, less time-consuming, specific and sensitive. Methods comparison revealed that gas chromatography is better than traditional titration in terms of method operability, accuracy and specificity, showing good application value.

Objective:To develop a method for determining deoxynivalenol in four kinds of traditional Chinese herbal medicines. Methods:After being extracted by water, purified by an immunoaffinity column, deoxynivalenol was analyzed by LC-MS-MS. Results:The calibration curve was linear within the range of 2-50 ng·ml-1 for deoxynivalenol. The recovery was 68. 7%-88. 3%. Conclusion:The method is simple, sensitive and accurate in the determination of deoxynivalenol in Semen Ziziphi Spinosae, Semen Sojae Praepara-tum, Semen Coicis and Fructus Psoraleae.

Objective:To improve the quality standard for Anweiyang capsules. Methods: TLC was used to identify Glycyrrhiza inflata Bat. Licochalcone A was determined by RP-HPLC. Using a C18 Column, the mobile phase consisted of acetonitrile-0. 1% phos-phoric acid(40:60), and the detection wavelength was at 376 nm. Results:The herb could be identified by TLC. For licochalcone A, the linear range was from 25. 563 to 1 533. 798 ng, and the average recovery was 99. 8%(n=9). Conclusion:The method is simple and accurate, which can be used to improve and control the quality of Anweiyang capsules.

Objective To evaluate the clinical significance of the detection of the Human Papilloma Virus (HPV) DNA typing in therapy of cervical diseases. Methods 780 cases have been studied. These cases which showed HPV-DNA positive and were diagnosed by biopsy as cervical cancer or cervical intraepithelial neoplasia( CIN Ⅰ-Ⅲ) were treated by operation or physical therapy. And 6 months and 12 months after the treatment,TCT and HPV DNA test were carried out. Results The prevalence of HPV-DNA types among the 780 cases descended from HPV 16 to 52,58,18,33 and 31. Detection rates of HPV-52 and 58 were highest among the patients with CIN Ⅰ. In patients with CIN Ⅱ,CIN Ⅲ,carcinoma in situ and invasive carcinoma,the positive rate of HPV-16 was obviously higher than other genotypes,and the difference was significant (P＜0. 01 ). 520 cases were followed-up after treatment,we found that HPV-DNA subsided within 3 months to 1 year in 432 cases. 88 cases still showed the HPV-DNA positive, among this group 48 cases were cytology diagnosed as normal or inflammation,but 14 cases were ASC-US,22 cases were LSIL and 4 cases were HSIL. Cytology abnormal cases were mere often detected in patients with persistent HPV-positive than in patients with HPV-negative. Conclusion Referring patients with cervical diseases the common HPV genotypes are 16,52,58,18,33 and 31. Especially HPV-16 are closely related with cervical cancer and high-level cervical intraepithelial neoplasis. HPV-DNA turn negative in most patients in 12 months after treatment. Persistent infection of HPV-DNA is related with the pathological changes persist.

A method of LC-QTOF/MS combining with chemical synthesis has been used to determine the structures of three novel bile acids from bear bile powder. Reference substances of tauroursodeoxycholic acid and taurochenodeoxycholic acid were oxidized by pyridinium chlorochromate. The products were analyzed by LC-QTOF/MS. Total 4 products including 3 isomers were predicted and identified according to the PCC oxidation theory and LC-QTOF/MS results. Bear bile powder samples were dissolved by methanol and analyzed by LC-QTOF/MS. Three unknown peaks were found and identified as 2-[[(3beta, 5beta)-3-hydroxy-7, 24-dioxocholan-24-yl]amino]-ethanesulfonic acid, 2-[[(5beta)-3, 7, 24-trioxocholan-24-yl]amino]-ethanesulfonic acid and 2-[[(5beta, 7beta)-7-hydroxy-3, 24-dioxocholan-24-yl]amino]-ethanesulfonic acid, separately, by matching their results with that of oxidation products above.

AIM: The multi-residues method was used to determine organophosphorus pesticides in traditional Chinese herbal medicines (TCHMs).METHODS: Fifty three pesticides were extracted by high-speed homogenization,and then cleaned sequentially by C_(18) and Carb/NH2 solid phase extraction (SPE) cartridges.The residues were simultaneously identified and quantified by GC-FPD equipped with dual tower,dual column and two FPD detectors.RESULTS: The analytical performance was demonstrated by the analysis of 6 TCHMs samples extracts,spiked at three concentration levels for each pesticide.In general,the recoveries ranging from 70% to 120%,with relative standard deviations (RSDs) less than 15%,were obtained.The limit of detection (LOD) for most of the targeted pesticides tested was below 0.01 mg/kg.CONCLUSION: The method has good extraction efficiency,purification effect and good reproducibility,which can be applied to the determination of organophosphorus pesticide residues in the routine analysis of TCHMs.

Objective To study the clinical and pathological characteristics of HPV-negative cervical cancer patients. Methods Retrospective analysis of 785 cervical cancer patients in Guangdong Women and Children Hospital from Jan. 2005 to Oct. 2015. By detecting high-risk HPV infection by flow-through hybridization genechip technique. Results (1) Among 785 cases of cervical cancer, 71 cases were negative for HPV infection tested by genechip technique, accounting for 9.0%(71/785), and the relative light units/cut off (RLU/CO) ratios of these 71 cases were less than 1 by hybird captureⅡ(HC-Ⅱ) methods. The results showed that the positive coincident rate of genechip technique detecting result with HC-Ⅱmethod was 100.0%(71/71). (2) There was no difference between 43 (60.6%) cases from 41-55 years old of 71 cases of HPV-negative patients and 392 (54.9%) cases from 41-55 years old of 714 cases of HPV infection patients (χ2=15.63, P=0.571). Among 71 cases of HPV-negative patients, 32 cases of patients with doing TCT, 6 (18.8%) cases for normal, 10 (31.2%) cases for atypical squamous cells of undetermined significance (ASCUS), 3 (9.4%) cases for atypical squamous cells cannot exclude high-grade squamous intraepithelial lesion (ASC-H), 3(9.4%) cases for low-grade squamous intraepithelial lesions (LSIL), 8 (25.0%) cases for hight-grade squamous intraepithelial lesions (HSIL), 2 (6.2%) cases for squamous cell carcinoma (SCC). And there were 391 cases of patients with doing thin-prep cytologic test (TCT) of 714 HPV infection patients, 60 (15.3%) cases for normal, 61 (15.6%) cases for ASCUS, 28 (7.2%) cases for ASC-H, 29 (7.4%) cases for LSIL, 164 (41.9%) cases for HSIL, 49 (12.5%) cases for SCC. There was no difference of TCT between HPV infection and HPV-negative patients (P>0.05). Among 70 cases from 71 patients with negative for HPV infection, there were 8(11.4%) cases in stage Ⅰa, 26 (37.1%) cases in stage Ⅰb1, 12 (17.1%) cases in stageⅠb2, 11 (15.7%) cases in stageⅡa, 10 (14.3%) cases in stageⅡb, 3 (4.3%) cases in stageⅢ-Ⅳ. There were 118(16.6%) cases in stageⅠa, 261 (36.8%) cases in stageⅠb1, 72 (10.1%) cases in stageⅠb2, 152 (21.4%) cases in stageⅡa, 87 (12.3%) cases in stageⅡb, 20(2.8%) cases in stageⅢ-Ⅳin 710 cases of HPV infection patients, in which there were no difference of clinical stage between HPV infection and HPV-negative patients (P>0.05). Among 69 cases from 71 patients HPV-negative infection, there were 51 (73.9%) cases for squamous carcinoma, 13 (18.8%) cases for adenocarcinoma, 5(7.2%) cases for adenosquamous carcinoma;and 593 (87.2%) cases for squamous carcinoma, 38 (5.6%) cases for adenocarcinoma, 39 (5.7%) cases for adenosquamous carcinoma, 10 (1.5%) case for others were in 680 patients of HPV infection, in which there was significant difference of adenocarcinoma between HPV infection and HPV-negative patients (χ2=11.96, P=0.001). Conclusions Flow-through hybridization genechip technique is the method of high sensitivity to detect high-risk type HPV, as like HC-Ⅱ method. HPV-negative of cervical cancer occurs mainly in 41-55 years old. Adenocarcinoma incidence is significantly higher in HPV-negative cases than those patients with infection of HPV positive.