Fluorescence enhancement reaction of flavoxate hydrochloride (FX) in strong alkali solution was studied, the mechanism of the reaction was investigated, and a novel fluorimetric method for analysis of FX in drug sample was established. FX has no intrinsic fluorescence, but it can slowly produce fluorescence in strong alkali solution. Heating can promote the fluorescence enhancement reaction. In 3D fluorescence spectra of the decomposition product of FX, two fluorescence peaks, located respectively at excitation wavelengths λex/ emission wavelength λem =223/410 nm, and 302/410 nm, were observed. Using quinine sulfate as a reference, fluorescence quantum yield of the decomposition product was measured to be 0.50. The structural characteriza- tion and spectral analysis of the decomposition product reveal that ester bond hydrolysis reaction of FX is firstly occurred during heating process, forming 3-methylflavone-8-carboxylic acid (MFA), then a cleavage reaction of the γ-pyrone ring of MFA occurred, producing α, β-unsaturated ketone. This product includes adjacent hydroxyl benzoic acid group in its molecule, which can form intramolecular hydrogen bond under alkaline condition, so that increase the conjugate degree and enhance the rigidity of the molecule, and thereby cause fluorescence enhancement. Based on this fluorescence enhancement reaction, a fluorimetric method was proposed for the determination of FX. A linear calibration curve covered the concentration range 0.020 3-0.487 µg · mL. The regression equation was I(F) = 23.9 + 5357.3 c, with correlation coefficient r = 0.999 7 (n = 8), detection limit D = 1.1 ng · mL(-1). The method was applied to the analysis of FX tablets, with a spiked recovery rate of 100.2%. The reliability of the method was verified by a UV-spectrophotometric method.
Alkalies ; Calibration ; Chemistry, Pharmaceutical ; Flavoxate ; analogs & derivatives ; chemistry ; Fluorescence ; Limit of Detection ; Reproducibility of Results ; Solutions ; Tablets

To ensure the quality and safety of Panax notoginseng, a method for the simultaneous determination of 10 mycotoxins in Panax notoginseng was developed using ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with acetonitrile and purified by HLB multifunction cleanup column. The separation was performed on a Phenomenex Kinetex XB-C18 column by gradient elution using methanol and 5 mmol·L(-1) ammonium acetate as mobile phase. The targeted compounds were detected in MRM mode by mass spectrometry with electrospray ionization (ESI) source operated in both positive and negative ionization modes. The linear relationships of the 10 mycotoxins were good in their respective linear ranges. The correlation coefficients (r) ranged from 0.9981 to 1.0000. The LOQs of the 10 mycotoxins were between 0.15 and 8.6 μg·kg(-1). The average recoveries ranged from 73.8% to 107.0% with relative standard deviations (RSDs) of 0.10%-10.9%. The results demonstrated that the proposed method was sensitive and accurate, and suitable for the mycotoxins quantification in Panax notoginseng.
Chromatography, High Pressure Liquid ; Chromatography, Liquid ; Drug Contamination ; Mycotoxins ; analysis ; Panax notoginseng ; chemistry ; Tandem Mass Spectrometry

Objective A prospective randomized controlled trial was carried out to explore the best time of In-domethacin suppositories administration for the prevention of post-ERCP pancreatitis in high-risk groups. Methods 81 patients were enrolled in the study finally. Patients were randomized into group A (100 mg rectal Indomethacin suppositories was administrated immediately after ERCP), group B (100 mg rectal Indomethacin suppositories was administrated half an hour after ERCP) and group C (ERCP alone group, which did not give Indomethacin supposito-ries). The level of serum amylase, urine amylase, serum CRP, serum IL-6, serum TNF-α were measured before, 3 h, 24 h and 48 h after ERCP, and the incidence of PEP and hyperamylasemia were analyzed. Results There was 1 case (4.00%) of PEP in group A, 2 cases (5.41%) of PEP in group B and 5 cases (26.31%) of PEP in group C;the incidences of PEP of group A and group B were significant lower than that in group C (P < 0.05). There was 1 case (4.00%) of hyperamylasemia in group A, 5 cases (13.51 %) of hyperamylasemia in group B and 6 cases (31.6 %) of hyperamylasemia in group C, and the incidences of hyperamylasemia of group A and group B were significant lower than that in group C ( P< 0.05). Conclusion Administration of 100 mg Indomethacin suppositories immediately or half an hour after ERCP can effectively reduce the incidence of PEP and hyperamylasemia.

Objective To investigate how to improve test quality by monitoring and analyzing 15 clinical laboratory quality indicators from the National Health and Family Planning Commission .Methods Data were collected from clinical laboratory department of the First Affiliated Hospital of Kunming Medical University between January 2011 and August 2015.15 quality indicators were analyzed retrospectively , including the error rate of specimen type , the coefficient variation unqualified rate of internal quality control test, the reporting rate of critical value , et al.Results The monitoring results of quality indicators basically satisfied the quality goals , except that the median of turn around time in pre-analytical phase was not established, routine internal quality control was not conducted in some laboratory tests in analytical phase and the reporting rate and reporting timely rate of critical value should be further improved in post -analytical phase .Conclusion Medical laboratory quality system can be continuously improved by means of setting up the quality goals of 15 quality indicators referring to sub-specialty and laboratory tests , as well as automated monitoring, statistics and analysis in LIS.

Objective To investigate the clinical characteristics, diagnosis and treatment of acute mesenteric venous thrombosis(MVT) in the elderly. Methods The clinical features, diagnosis, treatments and prognosis of 10 aged cases with acute MVT were retrospectively analyzed. Results The chief complaints of the 10 cases were different degrees of abdominal pain, which not paralleled with abdominal signs. The accompanying symptoms were nausea, vomiting and bloody stools and so on. All of these patients were misdiagnosised as pancreatitis, appendicitis or intestinal obstruction and so on. diagnosis of two cases was confirmed by ultrasound, 8 by CT. At the same time, 2 cases underwent angiography examination. Of the 8 cases who underwent operation, 5 cases were cured, 3 cases died (1 died of toxic shock and 2 died of multiple organ failure ). Two cases underwent conservative intervention thrombolysis. Conclusions It is essential to improve the knowledge of acute MVT,especially its intricate clinical characteristics, high rates of misdiagnosis and mortality. Early proper diagnosis is crucial. The main treatment is operation and conservative intervention thrombolysis can be performed in the patients whose bowel has not necrosed yet.

Objective To evaluate the damage caused by high intensity ultrasound(HIU)on tumor micro- vessels.Methods Rabbit models of the VX_2 tumor were set up.The target hepatic carcinomas were treated with HIU,and the results were observed using hematoxylin-eosin(HE)staining,vascular endothelial cell biotinylated-ulex europaeus agglutininiⅠ(UEAI)immunohistochemical staining,tumor micro-vessel counts,and electron microscopy. Results Histological examination through HE staining indicated that HIU induced carcinoma vascularities with whole tumor tissue coagulative necrosis.The UEAI immunohistochemical staining of the target lesions treated by HIU was ne- gative,and complete tumor micro-vessel uhrastructure damage was observed under the electron microscope.Conclu- sion HIU can damage tumor micro-vessels thoroughly,in such way that it may inhibit tumor growth and metastasis.

Objective To find out the situation of household consumption of iodized salt in Hebei province so as to provide scientific basis for prevention and control of iodine deficiency disorders(IDD). Methods According to the "national iodine deficiency disorders surveillance program (Trial)", the county (city, district) was taken as a unit, township (town) and administrative villages were selected in accordance with the principle of systematic sampling, then households were chosen by random sampling to collect their edible salt in Hebei province from 2007 to 2009. Salt iodine content was detected by direct titration method. Results A total of 48 675, 48 448 and 48 756 salt samples were collected from 2007 to 2009, respectively. The consumption rate of qualified iodized salt from 2007 to 2009 was 91.16%, 91.96% and 96.17%, respectively. There were 24.6%(41/167)and 18.0%(30/167)counties with consumption rate of qualified iodized salt under 90% in 2007 and 2008, respectively. The percentage of counties with consumption rate of qualified iodized salt above 90% was 100.0%(167/167) in 2009. In general there was a significant differences in frequency distribution of consumption rates of qualified iodized salt among the three years(H = 10.778, P ＜ 0.01 ), and the difference was found significant between 2007 and 2009 as well as between 2008 and 2009(all P ＜ 0.05), but was not significant between 2007 and 2008(P ＞ 0.05). Conclusions The consumption rate of qualified iodized salt at household level increases annually from 2007 to 2009. By 2009,the consumption rate of qualified iodized salt in each county is more than 90%, which has reached the national standard stipulated in "the evaluation programs for fulfilling the goal of eliminating IDD at county level".

Adult ; Base Sequence ; Drug Resistance, Multiple, Viral ; Genome, Viral ; Hepatitis B virus ; genetics ; Hepatitis B, Chronic ; drug therapy ; virology ; Humans ; Male ; Mutation ; Phylogeny

Objective To investigate the effects of standardized tertiary rehabilitation (STR) on limb motor function (LMF) after stroke.Methods Eighty-two patients were divided into a primary cerebral infarction group (PCI group) and a primary cerebral hemorrhage group (PCH group),and then randomly further divided into experi- mental and control sub-groups.All patients received routine internal medicine treatment,supplemented with stand- ardized tertiary" rehabilitation in the experimental groups.All patients were assessed with the simplified Fugl-Meyer motor function assessment (S-FMMFA) at enrollment,and 1,3 and 6 months after their stroke.Results The scores of the experimental groups were higher than those of the controls.The experimental groups scores were 26.10% of normal at the time of the enrollment,and improved to 42.52%,65.62% and 83.71% by the end of the 1st,3rd and 6th month,respectively.The control groups started at 18.51%,and progressed to 24.85% ,37.24% and 45.84% over the same interval.Conclusion STR was associated with improved LMF scores of stroke pa- tients.

Objective To understand the status of drinking-water-borne endemic fluorosis and the effect of preventive measure in Hebei province, so as to provide a basis to prevent and cure the disease. Methods Thirtyeight affected counties(cities, districts) with drinking-water-borne endemic fluorosis were sampled by random sampling in Hebei in 2009. All affected villages in every county were divided into mild, moderate and severe endemic fluorosis areas and a village was randomly selected from each category of the area to carry out the monitoring of endemic fluorosis. Dental fluorosis of children aged 8 - 12 were examined and 6 copies of urine samples were randomly collected in each age group in the above-mentioned villages. Clinical skeletal fluorosis was diagnosed among adults aged 16 and over and 20 copies of urine samples were tested for fluorosis in every village.Results A total of 112 affected villages were investigated, among which the drinking water quality of 66 villages were improved and 46 villages were not improved. A total of 236 copies of water samples from the 66 villages were measured and the fluoride content ranged from 0.1 to 4.3 mg/L, among which 20 copies of water samples exceeded the fluorine standard of 1.2 mg/L, accounting for 33.3%. A total of 230 copies of water samples were collected in the 46 villages and the fluoride content ranged from 0.2 to 4.6 mg/L, among which 76.1% (35/46) of the water samples exceeded the fluorine standard of 1.2 mg/L. A total of 5169 children aged 8 - 12 were examined of dental fluorosis, the dental fluorosis rate was 36.43%(1883/5169) and the dental fluorosis index was 0.81. A sum of 71 497 adults aged over 16 years were examined, and the rate of skeletal fluorosis was 4.81%(3438/71 497), moderate or severe clinical detection rate of skeletal fluorosis was 1.56%( 1114/71 497). A total of 2876 copies of children urine samples and 2021 copies of adult urine samples were tested and the geometric mean of fluoride content was 2.30,3.32 mg/L, respectively. Conclusions The prevalence of dental fluorosis of children in the areas with improved water is less than 30% and the rate of dental fluorosis and skeletal fluorosis decline gradually with time.The rate of dental fluorosis and skeletal fluorosis increases with the increase of water fluoride in the water quality not improved areas. The endemic fluorosis is still comparatively serious in Hebei. The progress of improving water quality in the areas with endemic fluorosis should be accelerated and the acceptability of improved water should be enhanced.