Gas Chromatography-Mass Spectrometry ; methods ; Humans ; Malathion ; metabolism ; urine

Objective To investigate the operative method and clinical rusults of repairing and reconstruction for bone and skin defect at medial malleolus.Methods Form January,2013 to January,2015,11 cases of patients with malleolus complex tissue defect were treated.According to the degree of damage to the cases were divided into four types,according to the type,selected flap,blood vessels,nerves,tendon graft,flap series connection iliac bone flap graft to repair,or direct ankle fusion,amputation to therapy.The Iliac flap donor site remained part of the anterior superior iliac spine and rebuild muscle starting and ending point,the donor sites wound was closed by skin graft.Results Followed-up of 1-24 months,in addition to amputation and ankle fusion each one exception,the remaining 9 patients underwent ankle reconstruction to reserve ankle.One case acquired infection,other 8 patients healed well,had different degree of recovery of the ankle function,the ankle function had recovery in different degree.AOFAS ankle-hindfoot score system:excellent in 4 cases,good in 4 cases,and poor in 1 case.Conclusion Ankle complex tissue defect classification method can be used to guide us to select the treatment options.Iliac bone flap series consisting mainly of composite tissue transplantation is a viable method of the medial malleolus defect reconstruction.

Objective To label human VEGF targeted bevacizumab (avastin) with 111In and to evaluate the application of 111 In?DTPA?avastin SPECT imaging for tumor diagnosis. Methods DTPA?avastin was prepared by coupling with a bifunctional chelating agent, and then labeled with 111 In to obtain 111 In?DTPA?avastin. The stability and molecular integrity of the labeled radiotracer were studied. Human hepatoma cell ( BEL7404) bearing nude mice tumor model was employed for tumor targeting evaluation. Gamma imaging was acquired after intravenous injection of 18.5 MBq probe. At the end of the observation, animals were sac?rificed for bio?distribution study. Results 111 In?DTPA?avastin tracer was synthesized and purified to a?chieve a radiochemical purity yield above 98% and specific activity up to 185 GBq/nmol. Its stability in 5%BSA was optimal, and the radiochemical purity after incubation for 96 h was over 90%. Gamma imaging re?sults showed that the tracer possessed definite tumor targeting property. Its biodistribution was consistent with that of normal in vivo antibody metabolism while possessing a good tumor?targeting property with a relatively high uptake of (3.8±0.8) %ID/g in tumor tissues 96 h after injection. Conclusions 111 In?DTPA?avastin tracer has good physicochemical properties, in vivo stability and good VEGF targeted binding. 111 In?DTPA?avastin has potential to be a new molecular probe for SPECT imaging.

Objective To investigate skin manifestations and comorbidities of chronic arsenicosis due to conta?minated drinking water, and to explore their possible risk factors. Methods Data about demographic characteristics, skin manifestations and comorbidities were collected from 95 patients with chronic arsenicosis due to contaminated drinking water in Inner Mongolia, and retrospectively analyzed. A logistic regression model was established to analyze associations of skin manifestations and comorbidities with patients′ gender, age, age at onset of drinking of arsenic?contaminated water, arsenic concentrations in water and duration of arsenic exposure. Results Among the 95 patients, 77 had hyperpigmentation, 75 hypopigmentation, 93 palmoplantar keratoderma, 27 skin cancer, and 8 multiple skin cancer. Five patients were complicated by tuberculosis, 15 by hypertension, 2 by rheumatoid arthritis, 4 by cerebral infarction, 7 by coronary heart diseases, 3 by internal malignancy, 6 by hepatic cirrhosis and 2 by anemia. Logistic regression analysis revealed a significant correlation between hyperpigmentation and arsenic concentrations in water(OR=0.32, 95%CI=0.10-0.98;ORadjusted=0.27, 95%CI=0.08-0.90), between occurrence of hepatic cirrhosis and arsenic concentrations in water (OR=24.67, 95%CI=2.69-226.57;ORadjusted=22.51, 95%CI=2.38-213.11), and between occurrence of coronary heart diseases and duration of arsenic exposure(OR=6.41, 95%CI=1.09-37.88;ORadjusted=8.55, 95%CI=1.21-60.41). Conclusions There is a high incidence of aberrant pigment metabolism, palmoplantar keratoderma and skin cancer in patients with chronic arsenicosis due to contaminated drinking water. Different arsenic concentrations in water and duration of arsenic exposure seem to have different influences on the human body.

Objective To study antibacterial effect of formulas, borneol, honey, gentamicin in wet honey ice bedsores.Methods The third-stage infective bedsore model in rabbit were estabished with Staphylococcus aureus ( S.aureus) , Escherichia coli ( E.coli) , and Pseudomonas aeruginosa ( P. aeruginosa).The rabbits with bedsore were respectively compressed with gauze of honey+borneol, honey+gentamicin,borneol+gentamicin,borneol+gentamicin+honey, vaseline as control group.The strain identification and colony counts were observed before and after treatment.ResuIts The colony count of S.aureus, E.coli and P.aeruginosa in honey+borneol, honey+gentamicin, borneol+gentamicin, borneol+gentamicin+honey post-treatment was significantly higher than that of pre-treatment, respectively (P<0.05).The colony count of three strains in above four formulas post-treatment was significantly lower than that in vaseline group, respectively (P <0.05).The colony count of three strains in borneol +gentamicin +honey (original formula) post-treatment was significantly lower than that in the other formulas, respectively (P<0.05).ConcIusion The antibacterial effect of borneol+gentamicin+honey (original formula) is the best.

Objective To summarize the risk factors, the diagnostic and therapeutic approaches, and the outcomes of the ruptured primary hepatocellular carcinoma (PHC) occurred after transcatheter arterial chemoembolization (TACE) in order to make a further understanding of this complication. Methods The clinical data of 8 patients with ruptured PHC after TACE, who were encountered at the First Affiliated Hospital of Suzhou University during the period from Sep. 2007 to Sep. 2013, were retrospectively analyzed. Results A total of 1379 times of TACE were performed in 678 patients with PHC. Among the 678 patients, 8 developed rupture of PHC with bleeding after TACE. The overall incidence was 1.2%. The mean diameter of the tumors in the 8 patients was (11.5 ± 2.6) cm, ranging from 7.6 cm to 15.9 cm. All the lesions were located at the peripheral region close to the liver capsule, and most of them protruded outward. Five cases had coexisting portal hypertension. The average dosage of Lipiodol used in TACE was (14.9 ± 4.5) ml with a range of (8 - 20) ml. Of the 8 patients, emergency transcatheter embolization was carried out in 4 and medical management was employed in other 4. Seven patients died as all active emergency treatments failed. Only one patient, who had received emergency transcatheter embolization, survived the ruptured PHC. Conclusion Rupture of primary hepatocellular carcinoma after TACE is a rare, but very serious complication. Its occurrence may be related to lesion’s characteristics, such as large tumor size, superficial location and protrusion from the liver surface, etc. Besides, interventional management, e.g. without use of solid embolic material to enhance the embolization effect, may also be responsible for the rupture.

OBJECTIVE: To establish a method for analysis of related substances in biapenem with micellar electrokinetic capillary chromatography(MEKC). METHODS: In order to improve the separation selectivity, a zwitterionic surfactant, 3-(N, N-dimethylhexadecylammonium)-propanesulfonate(PAPS) was used. The optimal separation conditions were as follows: the total length of the capillary was 48.5 cm (the effective length was 48 cm), the buffer was 90 mmol•L-1 tris(hydroxymethyl)aminomethane (tris)-phosphate buffer containing 17 mmol•L-1 PAPS and 3 mg•mL-1 polyoxyethylene 23 lauryl ether (Brij 35), the applied voltage was 22 kV, and the capillary temperature was controlled at 30℃. Further more, the specificity, linearity, precision, repeatability, stability and durability were studied. The contents of related substances in biapenem commercial samples were analyzed. RESULTS: The MEKC method, which was a comparable analysis method to HPLC, successfully separated the adjacent impurities of biapenem by using the zwitterionic surfactant PAPS. The specific test showed that this method was especially suitable for the detection of biapenem dimers A, B and open-ring compound. CONCLUSION: In this method, MEKC with zwitterionic surfactant is for the first time applied to the analysis of related substances in biapenem (amphoteric drugs). It provides a feasible analysis method with high sensitivity, good specificity and reproducibility for the quality control of biapenem.

OBJECTIVE: To develop a suitable HPLC method combined with component preparation to analyze the related substances and effective contents in bacitracin.METHODS: The separation was performed on Agilent HPLC system with a Diamonsil Plus C18 column (4.6 mm×250 mm, 5 μm) using 50 mmol•L-1 ammonium formate (pH adjusted to 4.0 with formic acid) as mobile phase A and acetonitrile as mobile phase B at a flow rate of 1 mL•min-1 under gradient elution. The detection wavelength was set at 254 nm. The HPLC method was carried out by adjusting the pH of ammonium formate solution, the ratio of mobile phase and the solvent. Furthermore, the specificity, linearity, precision, repeatability, stability and durability were studied. The known components like bacitracin A, B1/B2/B3, C1/C2/C3 and F were collected by preparative HPLC according to the HPLC method for bacitracin in USP 40. They were positioned in ammonium formate-acetonitrile HPLC system.RESULTS: The established HPLC method was verified to be suitable for analyzing the related substances and effective contents in bacitracin. Baseline separation between the known components and adjacent impurities was achieved, especially the B1/B2. The elution positions of the known component were clearly defined. The contents of the known components in different batches of bacitracin were compared. More detailed sample information was provided in this research.CONCLUSION: The HPLC method can simultaneously analyze the related substances and effective contents in bacitracin, and is suitable for the quality control of the product.

OBJECTIVE: To establish an HPLC-MS/MS method to identify the unknown impurities in polymyxin B sulfate. METHODS: The analysis was performed on Agilent 1260-6550 Q/TOF-MS with a Diamonsil Plus C18 column(4.6 mm×250 mm, 5 μm). Mobile phase A was 0.01 mol•L-1 trifluoroacetic acid-acetonitrile(95:5), and mobile phase B was acetonitrile containing 0.1% formic acid. Mobile phase A and B were set at the volume ratio of 79:21 at a flow rate of 1 mL•min-1 under isocratic elution. The detection wavelength was set at 254 nm. ESI source was used. Positive ion scanning was conducted in the range of m/z 50-1 700 for MS and MS/MS. The unknown components were identified by comparing the MS and MS/MS with the known reference standards like polymyxin B1 and B2. The photochemical Paterno-Büchi reaction was performed using a low-pressure mercury lamp as the light source at emission wavelength of 254 nm with acetone/water(50/50, V/V) as the reaction solvent. RESULTS: The structures of seven unknown related substances in polymyxin B sulfate were identified. The most abundant impurity was identified to be vinyl polymyxin B1, for which the double bond was at the end of the fatty acyl residue. CONCLUSION: Vinyl polymyxin B1 is reported for the first time. The method provides a good idea for the identification of related substances in drugs.

The compatibility of kanamycin with sodium citrate for the formulation of kanamycin sulfate injection was determined, including optimization of the amount of sodium citrate in the injection and the sterilization process. An HPLC coupled with an evaporative light scattering detector (ELSD) was used to measure the amount of sodium citrate and the impurity profiles. A validated post-column derivatization HPLC coupled with a fluorescence detector (FLD) was used to determine the correlation between specific impurities in a domestic factory and sodium citrate, and then the formulation was evaluated by HPLC coupled with mass detector (MS) characterization of degradation products. The results show that the amount of sodium citrate in kanamycin sulfate injection from a domestic factory is about 40 times higher than that of the Meiji formulation. Several specific impurities can be detected in solutions heated under simulated sterilization conditions (121 ℃), which were correlated with the amount of sodium citrate. Impurities were characterized by HPLC-MS/MS, and data showed that the identified impurities were interaction products of kanamycin and sodium citrate. These results indicate that greater attention should be directed at formula optimization in domestic factories, as it is crucial to the safety and efficacy of the preparations. Drug-excipient chemical compatibility should also be evaluated in the development of pharmaceutical dosages forms especially when the active pharmaceutical ingredients have a primary amine group.