Detection of 14 sulfonate esters impurities of active pharmaceutical ingredients based on GC-MS/MS and LC-MS/MS / 药学学报

Two methods including gas chromatography tandem mass spectrometry (GC-MS/MS) and high-performance liquid chromatography tandem mass spectrometry (LC-MS/MS) were established to detect common alkyl sulfonates and aryl sulfonates genotoxic impurities. Four alkyl sulfonates and methyl benzenesulfonate were determined by GC-MS/MS using butyl methanesulfonate as the internal standard, the chromatographic column was HP-5MS UI (30 mm × 0.25 mm, 0.25 µm), the carrier gas was helium, the flow rate was 1.0 mL·min-1 in a constant flow mode, the sample inlet temperature was set to 250 ℃, the split ratio was 10∶1, and the initial temperature of the heating program was 80 ℃, maintained for 1 minute, and then increased to 240 ℃ at a heating rate of 30 ℃·min-1 for 2 minutes. The mass spectrometry detector was an electron bombardment ion source (EI source), the data collection condition was multi reaction monitoring mode (MRM), and method validation using the raw material of clinical drug citalopram hydrobromide as a sample. The results showed that the linear range of four alkyl sulfonates and methyl benzenesulfonate were good at 3-50 ng·mL-1 and 9-150 ng·mL-1, with a correlation coefficient of r > 0.999, The spiked recovery was 80%-120%. The detection limits were 1 and 3 ng·mL-1; Ten aryl sulfonates determined by LC-MS/MS, the chromatographic column was CSH Fluoro phenyl (100 mm × 2.1 mm, 1.7 µm), the mobile phase was methanol (B)-5 mmol·L-1 ammonium formate (D), with a flow rate of 0.2 mL·min-1, and gradient elution was performed. The gradient program (T/% B) was set as 0/20, 25/90, 35/90, 42/20. The mass spectrometer detector was electro spray ionization with positive ionization mode (ESI+), the data collection was in dynamic multi reaction monitoring mode (dMRM), and the method was validated using the raw material of the clinical drug citalopram hydrobromide as a sample. The results showed that the linear range of aryl sulfonates were good at 9-2 000 ng·mL-1, 3-100 ng·mL-1 and 0.9-30 ng·mL-1, respectively. The correlation coefficient r > 0.999, the spiked recovery was 80%-120%. The detection limits were 30, 1 and 0.3 ng·mL-1. Two detection methods did not detect potential sulfonate genotoxicity impurities in the above APIs. The established analytical methods are reliable and effective, which can provide reference for drug quality control and detection.

Comparision of Cardiac Output Measured by Transthoracic Echocardiography with Continuous Cardiac Output Measured by Pressure Recording Analytical Method

Background: Low cardiac output is a common complication following cardiac surgery and it is associated with higher mortality in the pediatric population. A gold standard method for cardiac output (CO) monitoring in the pediatric population is lacking. The present study was conducted to validate cardiac output and cardiac index measured by transthoracic echocardiography and Pressure recording analytical method, a continuous pulse contour method, MostCare Up in postoperative pediatric cardiac surgical patients. Materials and Methods: This was a prospective observational clinical study conducted at a tertiary care hospital. A total of 23 pediatric patients weighed between 2 and 20 kg who had undergone elective cardiac surgery were included in the study. Results: Spearman抯 correlation coefficient of CO between transthoracic echocardiography (TTE) and Pressure Recording Analytical Method (PRAM) showed of positive correlation (r = 0.69, 95% Confidence interval 0.59?0.77, P < 0.0001) Linear regression equations for CO between TTE and PRAM were y = 0.55 + 0.88x (R2 = 0.46, P < 0.0001). (y = PRAM, x = TTE), respectively. Bland? Altman plot for CO between TTE and PRAM showed a bias of ?0.397 with limits of the agreement being ?2.01 to 1.22. Polar plot analysis showed an angular bias of 6.55� with radial limits of the agreement being ?21.46 to 34.58 for CO and angular bias of 6.22� with radial limits of the agreement being ?22.4 to 34.84 for CI. Conclusion: PRAM has shown good trending ability for cardiac output. However, values measured by PRAM are not interchangeable with the values measured by transthoracic echocardiography.

Rapid identification of chemical constituents in Xuezhikang Capsule by UPLC-Q-TOF/MSE combined with the establishment of UNIFI MS database / 药学学报

An UPLC-Q-TOF/MSE technology coupled with UNIFI database was used to develop a rapid, high coverage, accurate and efficient chemical composition qualitative method for Xuezhikang Capsule. A UNIFI database was established utilizing compound name, formula, structure, following automatic matching with high-resolution mass numbers, isotope distributions, mass deviations, fragment ion matching, and chromatographic retention features in UNIFI database to achieve the qualitative results of natural products in Xuezhikang Capsules. Combined with manual confirmation, 82 chemical components were identified in Xuezhikang Capsules, and the MS2 fragmentation pathway of typical organic acids, flavonoids, monacrines, and monascus were analyzed to ensure accuracy of the LC-MS workflow. This study clarified the chemical substance basis of Xuezhikang Capsules by LC-MS technology, providing experimental data support for the identification of key quality attributes, quality control and consistency evaluation in the manufacturing process of Xuezhikang Capsules.

Characterization and application of exposure biomarkers of polycyclic aromatic hydrocarbons in diesel exhaust / 环境与职业医学

Diesel exhaust (DE), Group 1 carcinogen, is an important source of air pollutants. Studies show that DE exposure associates with elevated incidences of respiratory and cardiovascular diseases. The toxic effects of DE are closely related to its components. Polycyclic aromatic hydrocarbons (PAHs) are one of the main toxic components in DE and are often used as human exposure biomarkers to DE. However, the exposure assessment of DE using PAHs as biomarkers could be interfered due to the other sources of PAHs. Therefore, identification of highly specific and reliable PAHs sourced biomarkers of DE exposure has become a hotspot of current research. New biomarkers of DE may play an important role in determining human exposure to DE and establishing dose-response relationship of DE exposure and health outcomes of interest. This paper focused on current progress in terms of PAHs sourced biomarkers of human exposure to DE with the following aims: (1) to clarify the types of PAHs sourced biomarkers to DE; (2) to explore the applicability and limitations of PAHs sourced biomarkers for DE exposure assessment in occupational exposure and environmental exposure analysis; and (3) to summarize the analysis methods for PAHs sourced exposure biomarkers in human urine samples and compare the advantages and disadvantages of different analytical methods.

Advances in analytical methods for endogenous bile acids based on UPLC-MS/MS technology / 药学学报

Bile acids (BAs) are a group of endogenous steroid molecules that regulate lipid, glucose and energy metabolism. They play an important role in maintaining body homeostasis and physiological functions as key signaling molecules for host and gut microbial metabolism. The accurate characterization and quantification of BAs in vivo is of great importance in basic and clinical research. Over the past decades, enzymatic assay, enzyme-linked immunoassay, nuclear magnetic resonance (NMR), chromatography, and other related techniques have been developed and applied to the detection of BAs. The diverse structures of BAs, the existence of isomers and the complex matrix of biological samples pose great challenges for the detection of endogenous BAs. Ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) is a robust analytical technique that combines the rapid separation capacities of UPLC with the powerful structural identification capabilities of MS/MS, facilitating the more rapid separation, characterization and accurate quantitative of target analytes in biological samples. UPLC-MS/MS has been widely used in the quantitative analysis of BAs in recent years for its high selectivity, high sensitivity, and high accuracy. This paper summarized the biosynthetic pathways of BAs, sample pretreatment methods, common analytical detection techniques, and highlights the current status of the application of UPLC-MS/MS technology in the analysis of endogenous BAs over the past five years, to provide a reference for the accurate detection of endogenous BAs and further research development and application.

Research progress in bioanalysis and pharmacokinetics of liposome nanomedicine / 药学学报

Liposome nanomedicine is a new drug preparation with nano scale, which is encapsulated by lipid bilayer vesicle structure. As a drug delivery carrier, liposome has many advantages such as good biocompatibility, biodegradation in vivo and strong targeting. The application of liposome nano drug delivery system can improve the pharmacokinetic behavior and efficacy of some drugs in vivo to a certain extent, and reduce toxic and side effects. After liposome nanomedicine enter into the body, free drugs will be released, so there will be loaded drugs and free drugs in the body. Loaded drugs are drug repositories, free drugs are related to their efficacy and adverse reactions. Therefore, the pharmacokinetics study of liposomes should focus on both loaded drugs and free drugs. Quantitative analysis of free drugs, liposome particles and their materials is a big challenge. The bioanalysis and pharmacokinetics of liposome nanomedicines will be introduced and discussed in this review. We hope this review will provide a reference for the development of liposome nanomedicine.

Research progress in measurement methods for210Po and 210Pb in environmental samples / 中国辐射卫生

210Po and 210Pb exist widely in nature, and they have strong toxicity and strong ionization ability, which can cause continuous harm to human health. Therefore, it is of great significance to determine the activity concentrations of 210Po and 210Pb in environmental samples and to evaluate their harmful effects on human health. This article reviews the research progress in analytical methods and measurement techniques of 210Po and 210Pb in environmental samples.

Residual status, toxicity, and analytical method of banned pesticides in traditional Chinese medicines / 中国中药杂志

A total of 33 pesticides have been banned from Chinese medicinal materials and decoction pieces(plants) according to Chinese Pharmacopoeia(2020 edition). According to the chemical structures, they are mainly divided into seven categories: organophosphorus compounds, organochlorines, carbamates, amidines, sulfonylureas, phenylpyrazoles, and ethers. These banned pesticides exhibit neurotoxicity, reproductive toxicity, immune system toxicity, teratogenicity, carcinogenesis, and mutagenesis, seriously damaging human and animal health. They affect not only the quality and safety of traditional Chinese medicines and resulting products, but also their competitiveness in the international market. Due to the numerous varieties of traditional Chinese medicines and their complex substrates, it is necessary to establish a universal and highly sensitive method for pesticide residue detection. This review systematically summarized the residual status, toxicity, and analytical methods of banned pesticides in traditional Chinese medicines, and forecasted the prospects of different analytical techniques, so as to provide reference for further safety and risk assessment of banned pesticide residues in traditional Chinese medicines, thus ensuring the safe production of traditional Chinese medicines.

Application of capillary zone electrophoresis to determine second-generation H1 antihistaminic drugs, loratadine and rupatadine

Abstract The second generation of H1 antihistamines from the piperidine group are often used for treating allergic diseases due to their action on histaminic receptors, the primary mediator of allergy. Moreover, the antihistamines have anti-inflammatory action, mediated through platelet-activating factor blocking activity. A simple and rapid capillary zone electrophoresis method was developed and validated for the determination of loratadine (LOR) and rupatadine (RUP) in tablets. The analyses were carried out using a fused silica capillary of 50.2 cm (40 cm effective length), 75 µm i.d. The background electrolyte was composed of boric acid 35 mmol/L, pH 2.5. Voltage of 20 kV, hydrodynamic injection of 3447.3 Pa for 3s, temperature at 25 ºC, and UV detection at 205 nm were applied. Electrophoretic separation was achieved at 1.8 and 2.8 min for RUP and LOR, respectively. The method was linear for both drugs in a range of 50.0 to 400.0 µg/mL (r>0.99). The limits of detection and quantification were 46.37 and 140.52 µg/mL, for LOR and 29.60 and 89.69 µg/mL for RUP respectively. The precision was less than 5.0 % for both drugs. The average recovery was approximately 100 %. The proposed novel method can significantly contribute to the rapid detection of counterfeit products and in quality control of drug products containing antihistamines

Quantitative Analysis Of Pamabrom And Ibuprofen In Synthetic Mixture Using 1st Order Derivative Spectroscopy

Objective: The preliminary goal was to develop and validate 1st order derivative spectroscopic method for quantitative analysis of Pamabrom (PAMA) which is a xanthine diuretic and ibuprofen (IBU) which is a non-steroidal anti-inflammatory agent from its synthetic mixture. Methods: Analytical method was developed on Shimadzu double beam spectrophotometer equipped with UV probe 2.42 as software using methanol as solvent. Quantification of PAMA was carried out at zero cross over point of IBU that is 291 nm and for IBU, it was achieved at 278 nm which is zero cross over point of PAMA. Method was validated according to ICH Q2 R1 guidelines. Results: Method showed a linear response in the range of 2-12 µg/ml of PAMA and 20-120 µg/ml of IBU. Method was found to be accurate with recovery between 99.7–100.9 % for PAMA and 100.3–100.7 % for IBU. The method was found to be accurate and precise for quantitative analysis of PAMA and IBU. Conclusion: The developed method was successfully validated as per ICH Q2 R1 guidelines and was successfully applied for quantitative analysis of a synthetic mixture of PAMA and IBU.

Simultaneous Estimation Of Mometasone Furoate And Formoterol Fumarate By Hplc Method In Rotacaps

Objective: To develop and validate a simple and sensitive RP-HPLC method for the simultaneous determination of mometasone furoate (MOM) and formoterol fumarate (FOR) in pharmaceutical dosage forms. Methods: In RP-HPLC method, chromatographic separation was achieved using a mixture of a solvent system consisting of methanol–water (pH 3.5) in the ratio of 85:15 % v/v at a flow rate of 1 ml/min and detection was carried out at 225 nm. Results: The run time for the simultaneous estimation of drugs for the proposed method was 10 min as drugs eluted at 5.217 min (MOM) and 8.650 min (FOR). The linearity was found in the range of 33.33-299.97 μg/ml and 1-9 μg/ml for MOM and FOR, respectively. The values of limit of detection and limit of quantification were 3.634, 0.266 µg/ml and 11.014, 0.807 µg/ml, which indicates the sensitivity of the method for the estimation of MOM and FOR, respectively. The results of recovery studies for both the drugs were within the range i.e. 98.87-101.48 % which indicates the accuracy of the method. Relative standard deviation obtained from repeatability and reproducibility studies were less than 2% indicates the precision of the method. The proposed method was validated according to ICH guidelines. Conclusion: The proposed RP-HPLC method was found to be sensitive and precise because of the low LOD, LOQ and % RSD values (<2). The proposed work does not require acetonitrile and ion pairing reagent as compared to the reported methods. Therefore, method can be used preferably for routine analysis due to its simplicity and economic advantages.

Desenvolvimento e aplicação de método analítico para determinação de substâncias psicoativas em amostras biológicas de motociclistas empregando LC-MS/MS / Development and application of analytical method for psychoactive substances determination in biological samples of motorcyclists using LC-M/MS

Os acidentes de trânsito consistem em um grave problema de saúde pública, principalmente nos países em desenvolvimento. No Brasil, um dos recordistas mundiais nesse tipo de acidente, somente no ano de 2017 o número de mortos por essa causa foi de aproximadamente 35 mil, sendo que por volta de 12 mil eram motociclistas ou passageiros de moto. Dirigir sob efeito de substâncias psicoativas como drogas ilícitas e algumas classes de medicamentos pode aumentar significativamente o risco de ocorrências de acidentes automotivos. Pesquisas mostram que diversos fármacos psicoativos alteram a capacidade motora e cognitiva dos usuários, porém os únicos estudos brasileiros feitos com motociclistas avaliam a prevalência de uso de drogas ilícitas em usuários hospitalizados, não havendo assim trabalhos sobre o uso de outras substâncias psicoativas na população em geral de motociclistas. Visando a importância desse fato, o presente projeto avaliou a prevalência de drogas ilícitas (canabinoides, estimulantes e anfetaminas) e de fármacos psicoativos pertencentes às classes dos anti-histamínicos, relaxantes musculares, benzodiazepínicos e anorexígenos nas amostras de fluido oral de motociclistas na cidade de São Paulo. Para tal, foi desenvolvido um método analítico que utiliza a técnica de cromatografia líquida acoplada à espectrometria de massas. Além do desenvolvimento de um novo método analítico que poderá ser utilizado para o monitoramento de motoristas em geral, foram obtidos dados da prevalência do uso de drogas e medicamentos pelos motociclistas na cidade São Paulo, contribuindo assim para o desenvolvimento de medidas preventivas, políticas públicas e para o esclarecimento sobre os riscos de dirigir sob efeito de substâncias psicoativas

Traffic accidents are a serious public health problem, especially in developing countries. In Brazil, one of the world record holders in this kind of accident, in 2017 the number of death due to this cause was approximately 35 thousand, and nearly 12 thousand were motorcyclists or motorcycle passengers. Driving under the influence of psychoactive substances such as illicit drugs and some prescription drugs can significantly increase the risk of motor vehicle accidents. Researches shows that several psychoactive drugs alter the motor and cognitive capacity of users, but the few studies done in Brazil with motorcyclists evaluate the prevalence of illicit drug use in hospitalized users, thus there is no work on the use of other psychoactive substances in the general population of bikers. Considering the importance of this fact, the present project evaluated the prevalence of illicit drugs (cannabinoids, stimulants, and amphetamines) and psychoactive prescription drugs belonging to the classes of antihistamines, muscle relaxants, benzodiazepines and anorectics in motorcyclist's oral fluid samples in the city of São Paulo. Therefore, an analytical method has been developed using liquid chromatography coupled to mass spectrometry. A new analytical method was developed and validated and may be used to monitor drivers in general. Data about drugs prevalence and drug use by motorcyclists in São Paulo city were obtained contributing to the development of preventive measures, public policies and for clarification on the risks of driving under the influence of psychoactive substances

Research progress on analytical methods for blood steroid hormones / 中草药

Steroid hormone, the component of the endocrine system, plays an extremely important role in body development, immune regulation, and birth control. The accurate determination of steroid hormone is important for the prevention, diagnosis, and treatment of clinical endocrine diseases. In recent years, the determination of endogenous steroid hormones in biological samples has become increasingly widespread in clinical applications. In this article, the commonly used analysis methods of typical blood steroids from 2013 to 2018 were generalized and compared in order to provide more reference for the accurate determination of steroid hormone levels, and also provide more accurate basis for later clinical diagnosis and treatment.

Application of SWOT Analysis in Postoperative Rehabilitation of Breast Cancer / 中国康复理论与实践

@#Objective To analyze the effect of SWOT analytical method on the activities of daily living, shoulder mobility and quality of life of patients with aerobic training after oncoplastic breast surgery.Methods From January to December 2017, 80 patients after modified radical mastectomy for breast cancer in the breast surgery of our hospital were randomly divided into control group and observation group, with 40 cases in each group. Both groups were performed aerobic training of the affected extremity, and the observation group were performed with evaluations and detailed analysis on the internal strengths and weaknesses, and the external opportunities and threats using SWOT analytical method, so that the corresponding solutions to the rehabilitation exercise of the affected extremity could be used to instruct postoperative patients. They were assessed with Activities of Daily Living Scale (ADL), shoulder mobility and Functional Assessment of Cancer Therapy (FACT) three days, four weeks and eight weeks after operation.Results Three days after operation, there was no significant difference in the scores of ADL, shoulder mobility and quality of life between two groups (t<0.23, P>0.05). Four weeks and eight weeks after operation, the scores of ADL, shoulder mobility and quality of life were significantly better in the observation group than in the control group (t>6.14, P<0.001).Conclusion The application of SWOT analytical method in the analysis and guidance on the rehabilitation exercise of the affected extremity is beneficial to the postoperative rehabilitation of patients, in aspects of activities of daily living, shoulder mobility and quality of life.

Rapid and sensitive liquid chromatography-tandem mass spectrometric method for the quantitative determination of potentially harmful substance 5,5'-oxydimethylenebis (2-furfural) in traditional Chinese medicine injections

With the rapid development and wide application of traditional Chinese medicine injection (TCMI), a number of adverse events of some TCMIs have incessantly been reported and have drawn broad attention in recent years. Establishing effective and practical analytical methods for safety evaluation and quality control of TCMI can help to improve the safety of TCMIs in clinical applications. In this study, a sensitive and rapid high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method has been developed and validated for the quantitative determination of potentially harmful substance 5,5'-oxydimethylenebis (2-furfural, OMBF) in TCMI samples. Chromatographic separation was performed on a C18 reversed-phase column (150 mm × 2.1 mm, 5 µm) by gradient elution, using methanol-water containing 0.1% formic acid as mobile phase at the flow rate of 0.3 mL/min. MS/MS detection was performed on a triple quadrupole mass spectrometer with positive electrospray ionization in the multiple reaction-monitoring mode. The method was sensitive with a limit of quantification of 0.3 ng/mL and linear over the range of 0.3-30 ng/mL (=0.9998). Intra- and inter-day precision for analyte was <9.52% RSD with recoveries in the range 88.0-109.67% at three concentration levels. The validated method was successfully applied to quantitatively determine the compound OMBF in TCMIs and glucose injections. Our study indicates that this method is simple, sensitive, practicable and reliable, and could be applied for safety evaluation and quality control of TCMIs and glucose injections.

Research progress in cellular pharmacokinetics of nano-drug delivery systems / 药学学报

Nano-drug delivery systems (nano-DDS) are the hotspots of new drug delivery systems, which have many advantages, such as sustained and controlled release, targeting delivery. Traditional pharmacokinetics are difficult to predict the efficacy of drugs in vivo sometimes. It is urgently needed to extend the traditional pharmacokinetics studies to the cell/subcellular level and perform cell pharmacokinetic studies. The study on the pharmacokinetics of nano-DDS helps us to elucidate the mechanism of the actions of them in cells and guides us to design and develop nano-DDS more reasonably. This article summarizes the research content and methods on the cellular pharmacokinetics of nano-DDS, in order to provide an important reference for the early stage design of nano-DDS.

Another analysis method of VARK questionnaire results based on medical students in shanghai and it's empirical application / 中华医学教育探索杂志

Objective To make up for losing more information of original classification method of VARK questionnaire author ( especially for mixed styles ) , and put another analytical method based on"whether contain or not"principle and put it in empirical analysis and application. Methods The students in 4 medial colleges in Shanghai were surveyed with VARK 7.0 version in May, 2017. 4488 questionnaires were sent out and 4054 were effectively returned (90.3％). Statistical analyses were done with SPSS 20.0 software and the enumeration data were compared by chi-square test. Results ①The percentage of con-taining"V"type of Sensory Learning Styles in the whole students was 44.8％(n=1815), which had no statis-tical significance in different college levels, college sorts, genders, specialties and whether they were military academy students or not (χ2=5.958, 0.257, 1.386, 5.922, 4.146; P=0.051, 0.612, 0.239, 0.052, 0.042), while there was significantly statistical difference in data among students of different grades ( χ2=13.400;P=0.009).②The percentage of containing"A"type was 57.1％(n=2313), which had no statistical significance in different genders, specialties, grades and whether they were military academy students (χ2=0.536, 4.038, 8.274, 4.256;P=0.464, 0.133, 0.082, 0.039), while there was still statistical significance in different college levels and sorts (χ2=10.516, 10.447;P=0.005, 0.001). ③The percentage of containing"R"type was 53.9％(n=2185), which had no statistical significance in different college levels, college sorts, genders, specialties, grades and whether they were academy students (χ2=4.563, 0.417, 0.228, 0.433, 2.136, 0.863; P=0.102, 0.518, 0.633, 0.805, 0.711, 0.353). ④The percentage of containing "K" type was 64.8％ (n=2625), which had no statistical significance in different college levels, college sorts, specialties, grades and whether they were academy students (χ2=3.680, 3.391, 1.070, 9.708, 2.711; P=0.159, 0.066, 0.586, 0.046, 0.100), while there was still statistical significance in different genders (χ2=6.789;P=0.009).⑤According to original clas-sification of VARK questionnaire author, the percentage of mixed styles were at the most (57.0％), followed by"K"(17.3％), and then"A" (11.2％) and"R" (10.0％), and the least was"V" (4.5％), which had no sta-tistical significance in different college levels, college sorts, genders, specialties, grades and whether they were academy students (χ2=6.044, 18.045, 8.575, 5.955, 28.866, 11.622; P=0.196, 0.021, 0.073, 0.652, 0.025, 0.020). Conclusion The analytical classification method based on"whether to contain" is a scientific improvement and beneficial supplement to the original classification method of the author of VARK scale in practical application because it embodies the mixed style and contains more comprehensive and accurate information. And through the empirical test, it verifies that medical students have distinctive sensory learn-ing styles.

Development and validation of an HPLC-UV method for analysis of methylphenidate hydrochloride and loxapine succinate in an activated carbon disposal system / 药物分析学报

Unused medications have the possibility of being abused, causing serious harm to individuals who were not prescribed the drug. The Food and Drug Administration (FDA) recommends the proper disposal of unused prescribed medications to maintain safety and prevent environmental hazards. However, many of the current disposal techniques do not properly address safety. A drug disposal pouch containing granular activated carbon offers a unique disposal method to deactivate residual or expiredmedication in a convenient, effective, and safe manner. A robust and validated method for methylphenidate hydrochloride and loxapine succinate was developed using high-performance liquid chromatography (HPLC) and the deactivation efficiency of the disposal system was tested. Methylphenidate hydrochloride was analyzed on a C18 analytical column (250mm × 4.60mm, 100?) using acetonitrile-water (0.05％ (v/v) trifluoroacetic acid) as the mobile phase at a flow rate of 1.0mL/min with a run time of 15min and retention time of 7.8min. Loxapine succinate was separated on a C8100? (250 mm × 4.6 mm, 5 μm) column maintained at 25 °C using a flow rate of 1.0mL/min. The run time was 10min and the retention time of the drug was around 4.6min.Mobile phase was composed of acetonitrile and water (0.3％ triethylamine) at pH 3.0 as 40:60 (v/v). Reference standard solutions (100 μg/mL) for both drugs were prepared by dissolving in mobile phases. These methods provide good linearity (R2 = 0.999) over the range of 5–100 μg/mL for methylphenidate hydrochloride and 0.1–100 μg/mL for loxapine succinate. The assay methods were successfully applied to study the deactivation of these drugs.

O método analítico e as psicoses: do dispositivo freudiano à estrutura lacaniana / El método analítico y las psicosis: del dispositivo Freudiano a la estructura Lacaniana / The analytical method and the psychoses: from the Freudian device to the Lacanian structure

O artigo retoma as formulações teóricas de Freud acerca da diferença entre os campos da neurose e da psicose e dos limites do tratamento psicanalítico com psicóticos para, em seguida, apresentar as contribuições de Jacques Lacan à temática da psicose, no que alude à sua diferença estrutural, seu mecanismo específico e direção do tratamento. Demarca-se com o recorte teórico, uma revisão bibliográfica sobre o período a partir do qual Freud deixa de conceber a psicose pelo paradigma da neurose e em que o retorno efetivado por Lacan a Freud, com base em suas apropriações da linguística e da antropologia estrutural, deu centralidade à determinação do sujeito pela linguagem, à valorização do simbólico; permitindo com isso novas possibilidades para o tratamento da psicose

El artículo retoma las formulaciones teóricas de Freud acerca de la diferencia entre los campos de la neurosis y de la psicosis y de los límites del tratamiento psicoanalítico con psicóticos para en seguida, presentar las contribuciones de Jacques Lacan a la temática de la psicosis, lo que se refiere a la diferencia estructural, al mecanismo específico y a la dirección del tratamiento. Se demarca con el recorte teórico, una revisiónbibliográfica sobre el período a partir del cual Freud deja de concebir la psicosis por el paradigma de la neurosis y en que el retorno hecho efectivo por Lacan a Freud, con base en sus apropiaciones de la lingüística y de la antropología estructural, le da la centralidad a la determinación del sujeto por el lenguaje a la valorización de lo simbólico, permitiendo con ello, nuevas posibilidades para el tratamiento de la psicosis

This article takes up Freud's theoretical formulations about the difference between the neurosis and psychosis fields and the psychoanalytical limitations treatment with psychotic to, then, submit the Jacques Lacan's contributions to the psychosis theme, as referred to their structural differences, their specific mechanism and treatment direction. It is delimited with the theoretical framework, areview on the period from which Freud fails to conceive the psychosis by the neurosis paradigm and the return effected by Lacan to Freud, based on their appropriation of linguistics and anthropology structural, gave centrality to the subject determinationby the language, the symbolic appreciation; thereby providing new possibilities for the psychosis treatment

Determinación de Levetiracetam en suero humano por cromatografía líquida con detección de arreglo de diodos / Levetiracetam determination in human serum by liquid chromatography with diode array detection / Determinação de Levetiracetam em soro humano por cromatografia líquida com detecção de arranjo de diodos

Se desarrolló y validó un nuevo método analítico para determinar Levetiracetam (LEV) en suero humano utilizando cromatografía líquida de alta resolución (HPLC) con detección de arreglo de diodos. El procedimiento es sencillo, puede ser incluido en la rutina del laboratorio y prestar servicio tanto en el monitoreo terapéutico como en la urgencia. El método incluye las siguientes etapas: extracción líquido-líquido con diclorometano y evaporación de la fase orgánica, la droga se reconstituye con fase móvil, se inyecta en el cromatógrafo y se detecta a 205 nm. El tiempo de retención de LEV es de 5 minutos y no presenta interferentes con respecto a otras drogas comúnmente prescriptas con Levetiracetam. La curva de trabajo presentó un rango de linealidad entre 5,2 y 82,9 μg/mL, un límite de detección y cuantificación de 0,8 μg/mL y 2,7 μg/mL, respectivamente. La recuperación fue del 99,8%.

A new analytical method for Levetiracetam (LEV) determination in human serum was developed and validated by high performance liquid chromatography (HPLC) with diode detection. It is a simple methodology that can be included in the laboratory routine and can be useful in both therapeutic drug monitoring and emergencies. The drug extraction is performed through a liquid-liquid extraction with methyl chloride. Subsequently, the organic phase is evaporated, reconstituted with the mobile phase, and injected in the chromatograph to be detected at 205 nm. LEV retention time is 5 min and it does not show interference with respect to other drugs commonly prescribed with Levetiracetam. The work curve showed linearity between 5.2 and 82.9 μg/mL and a detection and quantification limit of 0.8 μg/mL and 2.7 μg/mL, respectively, while the recovery was of 99.8%.

Foi desenvolvido e validado um novo método analítico para determinar Levetiracetam (LEV) em soro humano, utilizando cromatografia líquida de alta eficiência (HPLC) com detecção de arranjo de diodos. O procedimento é simples, pode ser incluído na rotina do laboratório e prestar serviço tanto na monitorização terapêutica quanto na urgência. O método inclui as seguintes etapas: extração líquido-líquido com diclorometano, e evaporação da fase orgânica, o fármaco é reconstituído com fase móvel, é injetado no cromatógrafo e detectado a 205 nm. O tempo de retenção de LEV é de 5 minutos e não apresenta interferentes com relação a outras drogas, comumente prescritas com Levetiracetam. A curva de trabalho apresentou um intervalo de linearidade entre 5.2 a 82.9 μg/mL, um limite de detecção e quantificação de 0.8 μg/mL e 2.7 μg/mL respectivamente. A recuperação foi de 99.8%.