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@#Objective To develop and verify a method for determination of cyanide residues in polysaccharide-protein conjugate vaccines based on flow injection analysis(FIA)with amperometric detector.Methods After removing macromolecular substances in the samples by ultrafiltration,the cyanide residues were determined by a 3700 automatic chemical analyzer with the injection time of 35 s,injection volume of 200 μL,pump speed of 40%,sample cycle time of 140 s,ultraviolet wavelength of 312 nm and an Ampere detector.The developed method was verified for the specificity,matrix effect,linear range,limit of detection(LOD),limit of quantitation(LOQ),accuracy,presicion and stability.The cyanide residues in the polysaccharide derivative bulk(13 batches)and conjugate bulk(21 batches)of Haemophilus influenzae type b conjugate vaccine and group A and C meningococcal conjugate vaccine produced by 5 manufacturers were determined by the developed method.Results Blank samples showed no interference to detection;The recoveries of the matrix effector solution of Haemophilus influenzae type b conjugate vaccine polysaccharide derivative and conjugate bulk,group A and C meningococcal conjugate vaccine polysaccharide derivative and conjugate bulk were 97.4%,102.4%,96.8% and 99.8% respectively,with all CV values less than 15%;In the range of 0.312 5 ～ 80 ng/mL,cyanogroup concentration showed a good linear relationship with peak height with a regression equation of y = 133.13 x + 57.556,R2= 0.999 1;The LOD was 0.2 ng/mL,and the LOQ was 0.6 ng/mL.The average recoveries of the control solution were 108.9%,106.5%,103.5% respectively with RSD value of 6.4% in the groups added with 5,10 and 20 ng/mL of cyanogroup and the CV values of precision verification were all less than 15%;The average concentrations of the control solution injected 20 times continuously were 76,38,18and 5 ng/mL with all CV values less than 15%,when cyanogroup concentration was 80,40,20 and 5 ng/mL,respectively.Cyanide residues were detected in 13 batches of derivative bulk samples,while not in 2 batches of 21 batches of polysaccharide conjugate bulk samples,and were detected in the others.Conclusion The developed method had good accuracy,precision and stability,which might be applied to the quantitative determination of cyanide residues in polysaccharideprotein conjugate vaccines.
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Objective To establish a catalytic spectrophotometric method for determination of iodine in water without the use of highly toxic arsenic reagents with good precision and accuracy.Methods A new flow injection catalytic spectrophotometry method for determination of iodine in water was established by combining flow injection analysis (FIA) with a new catalytic spectrophotometry for determination of iodine with no need of arsenic reagent.The standard curve linearity,sample detection limit,precision and accuracy of different iodine content ranges (0-250,0-1 200 μg/L) were tested.The test result was compared with that of the arsenic-based catalytic spectrophotometry recommended by the iodine deficiency disorders monitoring program in China (recommended monitoring method).Results A calibration relation of C =aA2 + bA + d (C:iodine concentration,A:measuring absorbance peak area from FIA) of the new method existed in the range of 0-250 and 0-1 200 μg/L.The linear correlative coefficient were both 0.999 9.The detection limit for iodine in water was 0.3 μg/L.The FIA peak shape of the sample tube with the lowest content is determined,and the sensitive iodine signal is detected.The water samples with different iodine content ranges were determined in parallel for 6 times,and the coefficient of variation (CV) was 0.2％-2.7％;the recoveries ranged from 95.0％ to 105.0％,and the total average recovery was 100.3％.The measured values of water iodine standard material GBW 09113e [(8.2 ± 1.2) μg/L] and GBW 09114d [(62.0 ± 6.0) μg/L] in the standard curve of different iodine contents were all within the uncertainty range of the given value.There was no significant difference between the results of recommended monitoring method and the new method (t =0.781,P ＞ 0.05).Conclusions The new method for measuring water iodine has a wide standard curve range,high sensitivity,and good precision and accuracy.The instrument is easy to operate,and no need for toxic arsenic reagent.The method is a reliable method for water iodine detection.
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Objective To establish a catalytic spectrophotometric method for determination of iodine in urine without the use of highly toxic arsenic reagents and with good precision and accuracy. Methods Combined flow injection analysis (FIA) with new catalytic spectrophotometry, a new method for determination of iodine with no need of arsenic reagents was developed by the author. An ammonium persulfate digestion-flow injection catalytic spectrophotometry for determination of iodine in urine was established. Standard serial solutions and urine samples were all digested by ammonium persulfate before testing. The standard curve linearity in the range of 0-1200μg/L, detection limit,precision and accuracy in determining urinary iodine were tested. Results A good calibration relation of C=aA2+bA+d (C:iodine concentration,A:measuring absorbance peak area from FIA) of the newly developed method existed in the range of 0 - 1200 μg/L. The linear correlative coefficient was 0.9998. The FIA analysis speed was 60 samples per hour. The detection limit for urinary iodine was 7.1μg/L. Precision:The intra-assay coefficients of variation (CV) were 0.3％ - 3.0％ (n = 6) when measuring 9 urine samples with iodine concentration of 61.8-806.8μg/L;the intra-assay CV were 0.2％-1.7％(n=6) when measuring 5 urinary iodine national standard materials with iodine concentration of 76.9 - 883.0 μg/L; the inter-assay CV were 1.0％ - 1.2％ when measuring 6 batches of 3 urinary iodine national standard materials with iodine concentration of 76.9 - 232.0 μg/L. Accuracy:The average recovery rate was 98.3％ with a range of 91.2％ - 104.6％ when measuring 20 urine samples with iodine concentration ranged from 18.9 to 807.1 μg/L. The test results of 5 urinary iodine national standard materials were all within the given value range and the relative deviations ranges were-2.9％-0.7％. No significant difference was found between the results of the 48 urine samples determined by the current standard method (WS/T 107.1-2016) and the new method (t=0.029, P>0.05). Conclusions The new method has a wide standard curve range, high sensitivity, good precision and accuracy, and is simple and easy to operate, with automatic sampling, rapid analysis, and no need for toxic arsenic reagent which is difficult to obtain and can pollute the environment. The method is suitable for widely application and can be used as a reliable technical method for urinary iodine detection.
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The lymphatic system plays an important role in human health and disease. In addition to a role in the immune response, the lymphatics can also serve as a pathway for cancer metastasis.Head and neck squamous cell carcinoma (HNSCC) is one of the most common cancers.In the case where the primary focus has been controlled, cervical lymph node metastasis is one of the most important factors affecting the prognosis of head and neck cancer.Thus, understanding the anatomy of the lymphatic system is of paramount importance in predicting cancer metastasis and to perform proper lymph node dissection in cancer patients.The objective of this review is to summarize current imaging approaches that facilitate both basic science and clinical investigations of lymphatic vasculature.Mutation analysis of the laryngeal lymphatic system may provide a theoretical basis for the diagnosis and treatment of HNSCC.
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Objective To establish a method for automatic determination of iodine content in drinking water by flow injection analysis (FIA) without arsenic. Methods In the dilute nitric acid solution, iodide ion in appropriate amount of nitrous acid solution could catalyze the orange red iron thiocyanate complex fade, and the use of this method combined with flow injection analysis technology formulated a flow injection method, and experimental conditions of the method were optimized. The linear relationship and linear range of the standard curve, the detection limit, the precision and the accuracy of the sample determination were implemented under the optimized conditions. Results The optimum concentration of potassium thiocyanate solution (0.15 mol/L) and sodium nitrite was 27.30 ml and 8.00 g/L, respectively, by series of experimental studies. Under the condition, the linear range of the standard curve was 0-500μg/L, the standard curve linear relationship coefficient≥0.9990;method detection limit was 5.94μg/L; in precision experiment of low, medium and high concentrations of iodine, the coefficients of variation were 1.19%, 1.92%and 2.06%;in accuracy test, recovery rates were 100.49%-107.84%, and the total recovery rate was 103.15%. Conclusions The flow injection analysis method can be used to replace arsenic cerium catalyzed spectrophotometric detection of iodide in water; when the method is used in detection of the sample water iodide content of 0 - 500 μg/L, it has good precision and accuracy, automatic injection, automatic filling reagents and automatic detection system to reduce the burden on the staff, with arsenic-free reagents and reduced environmental pollution and the health hazards of the inspectors, which is suitable for iodine screening in high iodine areas.
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Spectrophotometric seawater pH measurement system is an urgent need of device due to its quick speed and high precision. Based on spectrophotometric method and flow injection analysis technique, an automated system for pH measurement of seawater was developed by integrating pump and valve flow path, LED light source, flow cell and spectrophotometer. This measurement system effectively avoided bubbles. The indicator of concentration gradient in the seawater sample was used to correct for the pH perturbation caused by the indicator, thus the operation of system was simple and convenient. with this system, only 1. 5 min was needed for a sample measurement with a precision of 0. 0013 pH units and an offset of 0. 0059 pH units. This system could be used for the rapid determination of pH of seawater collected by laboratory or research ship with high precision pH values.
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Introduction Chronic otomastoiditis causes pain, otorrhea, and hearing loss resulting from the growth of tissue within the normally hollow mastoid cavity. Objectives In this report, we used a lipidomics approach to profile major mastoid bone and tissue lipids from patients with and without otomastoiditis. Methods The bone dust created during mastoidectomy, as well as the mastoid tissue, was analyzed from seven patients. Bone dust was also collected and analyzed in an additional four otologic cases (parotidectomy requiring mastoidectomy). Samples were subjected to a modified Bligh/Dyer lipid extraction, then high-performance thin-layer chromatography (HPTLC), combined gas chromatography/electron impact-mass spectrometry (GC/EI-MS), and flow-injection/electrospray ionization-tandem mass spectrometry (FI/ESI-MSMS). Data were analyzed for identification and profiling of major lipid components. Results HPTLC revealed the presence of various lipid classes, including phosphatidylcholines, cholesterol, and triacylglycerols. GC/EI-MS analysis revealed the presence of cholesterol and several fatty acids. FI/ESI-MSMS analysis revealed a host of phosphatidylcholines, phosphatidylethanolamines, and cholesteryl esters. Conclusion We used a lipidomics approach to develop an efficient (both in time and tissue amount) methodology for analysis of these tissues, identify the most abundant and common lipid species, and create a base of knowledge from which more focused endeavors in biomarker discovery can emerge. In an effort toward improved patient categorization and individualized intervention, the ultimate goal of this work is to correlate these lipid molecules to disease state and progression. This is the first reported study of its kind on these tissues. .
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Humans , Mucocutaneous Lymph Node Syndrome/diagnosis , Mucocutaneous Lymph Node Syndrome/drug therapy , Coronary Aneurysm/etiology , Glucocorticoids/therapeutic use , Immunoglobulins, Intravenous/therapeutic use , Mucocutaneous Lymph Node Syndrome/etiology , Mucocutaneous Lymph Node Syndrome/physiopathology , Risk Factors , Tumor Necrosis Factor-alpha/antagonists & inhibitorsABSTRACT
El análisis químico día a día se acerca más a la automatización, buscando satisfacer las necesidades actuales de resultados rápidos y confiables. Los sistemas de análisis en flujo (FIA - Flow Injection Analysis) son una de las formas de aproximarse a la automatización. En este artículo se presentan los pasos necesarios para implementar una metodología FIA, para la determinación de Pb(II) en agua, partiendo de la revisión de los procedimientos clásicos y describiendo detalladamente los pasos necesarios para implementar la técnica de análisis en flujo. El trabajo produjo un método de análisis de Pb en agua que usa ditizona disuelta en isopropanol (agente cromogénico), en presencia de bromuro de cetiltrimetil amonio (CTAB), para solubilizar en agua el complejo, cuyas características más sobresalientes fueron: volumen de inyección de muestra de 81,7 µL, velocidad de flujo de 8,0 mL/min, tiempo de toma de espectros 1,4 s e intervalo lineal de 1,0 a 40 mg L-1.
Chemical analysis has evolved towards automation to satisfy the current requirements: fast analysis and certainty in the results. Flow injection analysis (FIA) is a way to reach automation. This work presents the necessary steps to obtain an optimized FIA methodology for the determination of Pb(II) in water by classic methods. The result was a FIA method to determinate Pb with dithizone (chromogenic agent) dissolved in iso-propyl alcohol, using cethyltrimethylammonium bromide (CTAB) to solubilize the complex. The main characteristics of the method were: injection sample volume 81.7 µL, flow 8.0 mL/min, spectra acquisition time 1.4 s and linear range 1 to 40 mg L-1.
Cada dia, a análise química é mais cerca da automatização com o fim de satisfazer as necessidades atuais de resultados rápidos e confiáveis. Os sistemas de análise em fluxo (FIA - Flow Inyection Analysis) são uma das formas de aproximação à automatização. Este artigo apresenta os passos necessários para implementar uma metodologia FIA para a determinação de Pb(II) em água, partindo da revisão dos procedimentos clássicos e descrevendo detalhadamente os passos necessários para implementar a técnica de análise em fluxo. Os resultado são um método de análise de Pb em água que usa ditizona dissolvida em isopropanol (agente cromogénico) na presença de bromuro de cetiltrimetil amônio (CTAB), usado para solubilizar o complexo em água. As características principais do método foram: volume de injeção de amostra de 81,7 µL, velocidade de fluxo de 8,0 mL min-1, tempo de aquisição de espectros de 1,4 s e intervalo linear de 0.9 a 40 mg L-1.
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No Brasil os dados sobre a utilização dos sulfitos pela indústria de alimentos e pesquisas sobre o seu consumo são escassos. Sendo assim, o objetivo desta pesquisa foi avaliar o nível de sulfitos em sucos de frutas e estimar seu consumo por escolares de 5ª. a 8ª. séries de escolas públicas, do ensino fundamental, do município de São Caetano do Sul-SP, Brasil. Foi aplicado questionário de freqüência de consumo de alimentos (QFCA) em 313 escolares, sendo 56,9 % do sexo feminino e 43,1 % do sexo masculino, com média de idade de 14,7 anos. Os alimentos sulfitados mais consumidos foram os néctares ou sucos de frutas, o açúcar refinado, as batatas fritas congeladas, o coco ralado, o suco de caju e as frutas secas e cristalizadas. Considerando os limites máximos permitidos (LMP) pela legislação brasileira, o consumo de SO2, em mg SO2/kg pc/dia, foi de 0,12 mg SO2/kg pc/dia, sendo que este valor médio corresponde a 17% da IDA (0,7 mg SO2/kg pc/dia). Já os resultados das análises dos sucos de frutas demonstram que a análise por injeção em fluxo (Flow injection analysis - FIA) modificada obteve resultados de sulfitos nas amostras analisadas com menor variação do que aqueles obtidos pelo método Monier-Williams (M-W) otimizado, e que nenhuma amostra ultrapassou os LMP.
In Brazil there are no data on use of sulphites by the food industry and research on their consumption by population. Thus, the objective of this research was to evaluate sulphites in fruits juices and estimate intake sulphites in a group of 5th 8th schoolchildren of public schools in São Caetano do Sul-SP, Brazil. It was applied a food frequency questionnaire (FFQ) at 313 schoolchildrens (56.9% female, 43.1% male and average age 14.7 years). Sulphited products identified were fruits juices, sugar, frozen chips, grated coconut, cashew juice and dried fruits. Considering maximum permitted levels (MPL) stabilished by Brazilian legislation, none of the students exceeded the ADI of 0.70 mg SO2/kg bw/day, with average of consumption of 0.12 mg SO2/kg bw/day (17 % of the ADI). The results of the fruits juices analysis demonstrated flow injection analysis (FIA) modified obtained better results than optimized Monier-Williams method (M-W) and no sample exceeded the MPL.
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Humans , Male , Female , Adolescent , Students/statistics & numerical data , Drinking , Juices , Sulfites/analysis , Adolescent Nutritional Physiological Phenomena , Food Additives/toxicity , Food Technology , Feeding BehaviorABSTRACT
Anionic surfactants in waters were determined using on-line double microporous membrane extraction-flow injection analysis method. This method was based on the extraction of the ion-association complex (λ_(max)=650 nm) which formed from methylene blue cation and anionic surfactants. The on-line double microporous membrane liquid-liquid extraction phase separators were adopted. Optimization of variables of the flow injection manifold, groove mechanical dimension of the phase separator, and pore size of the membrane was performed. The proposed method had a linear range of 25.0-1000.0 μg/L(r≥0.999). The detection limit was 4.28 μg/L. The relative standard deviation(n=7) of different concentration was 0.7%-6.0%. The recovery was between 96%-110% and the sample throughput was 18 h-1. The method was applied to the analysis of standard Reference materials with satisfactory results. For practical application, two water samples were analyzed with the established method.
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El paraguat es un herbicida que pertenece al grupo de los biperidilos. Su determinación cuantitativa en orina es muy importante para diagnosticar la supervivencia de pacientes intoxicados. Muchos centros hospitalarios utilizan pruebas semicuantitativas para la determinación de paraquat en muestras biológicas. Sin embargo, éstas suelen carecer de precisión y exactitud. Por tanto, el desarrollo de métodos alternativos simples, exactos, precisos y accesibles podría resultar muy útil en instituciones hospitalarias. Sobre la base de estas consideraciones, se propone un método de análisis por inyección en flujo y detección espectrofotométrica para la determinación cuantitativa de paraquat en muestras de orina. La determinación se basa en la formación de un producto coloreado (600 nm) posterior a la reducción de paraquat con glucosa en un medio alcalino, mediante un sistema en línea. Bajo las condiciones óptimas de operación, la ley de Beer se cumple en el intervalo 1-50 µg mL-1 de paraquat con un coeficiente de correlación >0,999. La frecuencia de análisis fue de 12 h-1 con una desviación estándar relativa del 2,8% para una solución muestra que contiene 10 µg mL-1 de paraquat (n=3). El estudio de recuperación osciló entre 97,9 y 102,1%. El método analítico fue aplicado satisfactoriamente al análisis de muestras de dos pacientes intoxicados con paraquat.
Paraguat is a herbicide beloging to the bipyridinium group.The quantitative determination of paraquat in urine of humans is very important to diagnose survival of intoxicated patients. Many hospitals use semi-quantitative tests for determining paraquat in biological samples. However, they often lack precision and accuracy. Therefore, the development of simple, precise, accurate and accessible alternative methods could be very useful in hospital institutions. Based on these considerations, a flow-injection spectrophotometric procedure is proposed for paraquat determination in urine samples. The determination is based on the formation of a coloured product (600 nm) after on-line reduction of paraquat with glucose in alkaline medium. Under optimal conditions of operation, Beer's law is obeyed in a concentration range of 1-50 µg mL-1 of paraquat with a correlation coefficient >0.999. The analytical frequency was 12 h-1 and the relative standard deviation was 2.8% for a sample solution containing 10 µg mL-1 paraquat (n=3). Recovery studies were between 97.9 and 102.1%. The analytical method was satisfactorily applied in the analyses of samples from two intoxicated patients.
Subject(s)
Paraquat/urine , Paraquat/poisoning , Paraquat/toxicity , Spectrophotometry/methods , Continuous Flow , Chemistry Techniques, Analytical/methods , HerbicidesABSTRACT
Objective To establish a method for the determination of aluminium in drinking water by flow injection analysis instrument.Methods In a hexamine buffer solution(pH=6.0),phenanthroline solution and ascorbic acid as the anti-interference agent,aluminium could react with chromazurol S solution and form a compound,of which maximum absorption was at 550 nm.Results The linear range for this method was 5-200 ?g/L.The correlation coefficient was 0.999 3,the detection limit of this method was 2.0 ?g/L,the recovery rates were in the range of 92.2%-108% and RSD were in the range of 2.5%-8.2%.Conclusion The flow injection method is simple,rapid,accurate and is applicable to the determination of aluminium in drinking water.
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Objective To establish a new non radioimmunoassay for detecting insulin. Methods We put together the techniques of chemiluminescent analysis, flow injection analysis and immunoassay and established a method,flow injection chemiluminescent immunoassay, for insulin determination using sandwhich procedure with the horseradish peroxdase (HRP) as label of antibody and using the detection system of synergistic enhanced chemiluminescence of para phenylpenol and sodium tetraphenylborate with HRP catalysed oxidation of luminol. Results Satisfactory results were obtained in the dynamic range 0.15～60.00 ?U with a relative coefficient of 0 997 2 ( P
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Objective To develop a stable and quick method to determine the urea in swimming pool water.Methods On the conditions of strong acid and calefaction,urea can react on antipyrine and diacetyl monoxime and become yellow which can be determined by colorimetric analysis in 450 nm with the ALLIANCE FUTURA continuous flow injection auto analysis system.Results Determined by this method,the linear range was 0.5-4.0 mg/L,the regression equation was y=0.077 5x+0.021 9,the correlative coefficient r=0.999,the detection limit was 0.07 mg/L.With residual chlorine of 0.3 and 3.0 mg/L,the recovery rates were 98.8%-104.0% and did not disturb the determination.The results determined by the present method were the same as those by the method in GB/T 18204.29-2000(Wilcoxon Signed Ranks Test:Z=0.051,P=0.959).Conclusion Determination of the urea in swimming pool water with continuous flow injection auto analysis,the sensitivity,accuracy and limit of determination can meet to the requirement,moreover,the analysis speed is faster,less reagent will be needed,the present method can be generalized in the laboratory that has the conditions.
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Objective To establish a simple,accurate and sensitive method for determination of cyanide in drinking water. Methods By means of using flow injection analysis instrument, the cyanide in drinking water was determined on-line. Results The data obtained by this assay accorded with Beer's Law, the range was 2.0-50.0 ?g/L, r≥0.999, the detection limit, relative standard deviation and recovery rate were 0.23 ?g/L, 2.5%-3.8% and 94.9%-98.7% respectively. The sampling frequency was 20 samples per hour. Conclusion The method for determination of cyanide in drinking water employed in the present paper is simple, accurate, sensitive and suitable for the analysis of large number of water samples.
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Objective: To establish a simple and accurate method for Chuanxinlian Tablets (Herba Andrographis). Methods:The contents of dehydroandrographolide in Chuanxinlian Tablets was determined by FIA. The detection wavelength was at 540nm. Results:The linear was 0.2～1mg?mL -1 , the average recovery was 101.7%, RSD was 0.7% , respectively. The sampling frequency was 120 samples?h -1 . Conclusion:The method is simple, rapid and stable. It is suitable for the analysis of this preparation.
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A sensitive and rapid flow injection analytical method for the determination of ascorbic acid has been developed, based on the reaction between iodine and ascorbic acid(VC) and the reaction between iodine and starch. The linear range of VC is 0-12ppm. Recoveries of 96-110% can be obtained. The method was applied to the determination of VC in medicines and foods with satisfactory results.
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A catalytic spectrophotometric method for determination of trace molybdenum by flow injection analysis has been established, based on the catalytic oxidation of potassium iodide by hydrogen peroxide in the presence of molybedenum (VI) and the iodine produced is coloured with starch. The linear range and detection limit for molybdenum (VI) were 0 to 0.4 ppm and 3.2 ppb. The method has been successfully applied to determine molybdenum in the grain, soil and hair.