Preparation and application of proficiency testing sample of myclobutanil and procymidone in apple powder / 上海预防医学

ObjectiveTo prepare pesticide residues in fruit matrix samples that meet the requirements of homogeneity and stability for the proficiency test. MethodsThe pollution-free apple was selected as the main raw material to prepare the pesticide residue proficiency test samples of myclobutanil and procymidone， and to evaluate the homogeneity and stability. The results of the proficiency test were assessed using robust analysis and Ζ value. ResultsThe homogeneity and stability of the reference materials met the relevant requirements. Among 109 laboratories participated in the proficiency testing， 107 （98.2%） laboratories had satisfactory results. Suspicious test results were reported only in two laboratories， one laboratory for each of the two assessment items. ConclusionAn apple powder matrix sample with pesticide residues is successfully prepared for proficiency test， and could provide an evaluation tool for pesticide residue testing laboratories.

Characterization of ethyl acetate and methanol extracts of Commiphora myrrha and evaluating in vitro anti-diabetic and anti-obesity activities

Diabetes mellitus is a clinical disease categorized by hyperglycemia. Reduction of gastrointestinal glucose absorptionthrough the inhibition of carbohydrate digesting enzymes is one of in vitro anti-diabetic therapeutic approach. Thisinvestigation aimed to estimate the in vitro anti-diabetic and anti-obesity activities for ethyl acetate and methanolextracts of Commiphora myrrha oleo-gum as well as the identification of the bioactive compounds. Commiphoramyrrha was extracted with methanol and ethyl acetate. The two extracts were used to evaluate their α-glucosidase,α-amylase, and pancreatic lipase inhibitory activities. Identification of the bioactive compounds of ethyl acetate wasanalyzed by GC-MS (gas chromatography-mass spectrometry). The results showed that the ethyl acetate extract hada stronger inhibition activity on α-amylase (IC50 = 54.60 µg/ml) and α-glucosidase (IC50 = 58.7 µg/ml) than methanolextract on α-amylase (IC50 = 124.01 µg/ml) and α-glucosidase (IC50 = 191.2 µg/ml). Also, ethyl acetate extract hada promising inhibitory effect on pancreatic lipase (IC50 = 107.8 µg/ml) than methanol extract (IC50 = 498.1 µg/ml).GC-MS analysis of ethyl acetate extract identified 31 compounds. Among them nobiletin (50.26%), metaproterenol(orciprenaline) (14.99%), morantel (8.86%), and tricetin (3.38%) were the main compounds. These findings provedthat C. myrrha has anti-diabetic and anti-obesity inhibition activity may be due to the bioactive compounds withinteresting medicinal properties.

Determination of Sevoflurane, Isoflurane and Enflurane in the air of workplace by gas chromatography / 中华劳动卫生职业病杂志

Objective@#To establish a solvent desorption gas chromatographic method for determination of Sevoflurane, Isoflurane and Enflurane in the air of the Workplace.@*Methods@#Sevoflurane, Isoflurane and Enflurane were collected with activated carbon tube and desorbed with dichloromethane, separated with DB-1 capillary columns, and then detected with flame ionization detector.@*Results@#The linearity ranges were 1.9-304.8 μg/ml for Sevoflurane, 2.1-300.4 μg/ml for Isoflurane and 1.7-305.2 μg/ml for Enflurane, The correlation coefficient was both >0.999. Their limits of detection were 0.6 μg/ml, 0.6 μg/ml and 0.5 μg/ml, and Their limits of quatification were 1.9 μg/ml, 2.1 μg/ml and 1.7 μg/ml, and their minimum detectable concentrations were 0.1、0.2 and 0.1 mg/m3 per 4.5 L of air. Their relative standard deviations (RSD) were 2.5%-3.0%, 2.3%-3.1% and 2.2%-3.0%. The average desorption efficiencies were 101.1%-103.3%, 100.7%-102.7% and 101.0%-102.9%. The sampling efficiency was both 100%. The breakthrough volume of 100 mg actived carbon was 3.7 mg, 3.4 mg and 3.4 mg. Sevoflurane, Isoflurane and Enflurane in activated carbon tube could be kept at least 10 days at room temperature without significant losses.@*Conclusion@#The method shows lower detection limit, high accuracy and precision. It is feasible for determination of Sevoflurane, Isoflurane and Enflurane in the air of workplace.

Análise da composição do óleo essencial de Croton tricolor como um modelo na criação de acordes em fragrâncias na indústria da perfumaria / Analysis of the Croton tricolor essential oil composition as a model in the creation of fragrance accords for the perfumery industry

O uso de óleos essenciais na indústria de fragrância tem crescido a cada ano. A indústria de cosméticos, em geral, tem buscado este tipo de ingrediente com o objetivo de agregar atributos únicos e melhores aos seus produtos e assim entregar, ao consumidor final, diferenciais que poderão valorizar suas formulações, além de simplesmente perfumar. O benefício de usar óleos naturais ou acordes de seus principais componentes em formulações de fragrâncias é que estes se tornam composições mais ricas, e em muitos casos, capazes de proporcionar perfumação prolongada ao produto, quando comparados àqueles sintetizados. A presença de compostos variados nos óleos, como terpenos e resinas, ajudam a promover singularidades à fragrância e até mesmo servem como inspiração às criações de produtos com descrições olfativas de produtos naturais. Croton tricolor (Euphorbiaceae), segundo avaliação inicial de um perfumista, apresentou excelentes características olfativas, o que facilitou seu uso nos estudos. A análise do óleo essencial de C. tricolor por cromatografia à gás com detector de ionização de chamas (CG/DIC) e cromatografia à gás acoplada à espectrometria de massas (CG/EM) permitiu quantificar e identificar seus principais marcadores, bem como utilizar estas informações para construção de acorde olfativo, reproduzindo o odor do produto natural. O óleo essencial de C. tricolor apresentou como principais componentes o biciclogermacreno (15,4%), espatulenol (10,5%) e o alfa-pineno (6,8%). A partir destes dados foi construído um acorde aromático que reproduziu o odor original, contendo alfa-pineno (7%), álcool fenetílico (5%), óleo de cedro (5%), óleo de laranja (0,5%), limoneno (1%), eucaliptol (0,5%) e nerolidol (0,3%). Os compostos majoritários, biciclogermacreno e espatulenol, não foram adicionados por não serem disponíveis comercialmente, por isso, usaram-se outras matérias-primas semelhantes em perfil olfativo e ofertadas no mercado, como foi o caso do uso de álcool fenetílico, óleo de cedro e óleo de laranja na criação do acorde. Os resultados evidenciaram que a criação de acordes é um método economicamente viável para a reprodução de odores naturais que podem ser utilizados em formulações de fragrâncias, além de ajudar a resolver problemas na produção e comercialização de óleos essenciais como, sazonalidade e reprodutibilidade

The use of essential oils in the fragrance industry has grown every year. The cosmetics industry has generally sought this type of ingredient, with the aim of providing its products with differentiated benefits (unique and better attributes), and thus delivering to the final consumer a differential that can enhance their formulations, besides simply perfuming their products (theirs). The benefit of using natural oils or accords of their major components in fragrance formulations makes them richer, and in many cases capable of providing prolonged perfuming to the final product when compared to synthesized products. The presence of varied compounds in the oils, such as terpenes or (and) resins, helps to promote differentiated fragrance characteristics (singularities/peculiarities to the fragrance), or (and) even to serve as inspiration for product creations with olfactory descriptions of natural products. Croton tricolor (Euphorbiaceae), accordingly to an initial evaluation of a perfumer, presented excellent olfactory characteristics, which facilitated its use in the studies. The analysis of the C. tricolor essential oil by gas chromatography with flame ionization detector (GC/FID) and gas chromatography coupled to mass spectrometry (GC/MS) allowed to quantify and identify their main markers, as well as to use this information to construct an olfactory accord that reproduces the odor of natural products. The C. tricolor essential oil had as main components bicyclogermacrene (15.4%), spathulenol (10.5%) and alpha pinene (6.8%). From these data, an aromatic accord was created reproducing the original odor containing alpha pinene (7%), phenethyl alcohol (5%), cedar oil (5%), orange oil (0.5%), limonene (1%), eucalyptol (0.5%) and nerolidol (0.3%). Some of the major compounds, bicyclogermacrene and spatulenol, could not be added because they were not commercially available. In these cases (therefore), other products (raw materials) with similar olfactory characteristics (olfactory profile) and commercially viable (offered on the market) were used, such as the use of phenethyl alcohol, cedar oil and orange oil in the accord creation. The results showed that accord creation is an economically viable method for the reproduction of natural odors that can be used in fragrance formulations and may help to solve problems that exist in the production and commercialization of essential oils such as production seasonality and reproducibility

Development and evaluation of an inhalation chamber for in vivo tests

ABSTRACT The bioavailability, toxicity, and therapeutic efficacy of a drug is directly related to its administration route. The pulmonary route can be accessed by inhalation after fumigation, vaporization or nebulization. Thus, pharmacological and toxicological evaluation accessed by an apparatus specifically designed and validated for this type of administration is extremely important. Based on pre-existing models, an inhalation chamber was developed. This presents a central structure with five animal holders. The nebulized air passes directly and continuously through these holders and subsequently to an outlet. Evaluation of its operation was performed using clove essential oil, a nebulizer, and a flow meter. The air within the chamber was collected by static headspace and analyzed by gas chromatography with a flame ionization detector. For this purpose, a 2.5 minutes chromatographic method was developed. The air flow in each of the five outputs was 0.92 liters per minute. During the first minute, the chamber became saturated with the nebulized material. Homogeneous and continuous operation of the chamber was observed without accumulation of volatile material inside it for 25 minutes. The inhalation chamber works satisfactorily for in vivo tests with medicines designed to be administrated by inhalation.

Quantitation of ethyl glucuronide in serum & urine by gas chromatography - mass spectrometry.

Background & objectives: Alcohol misuse has now become a serious public health problem and early intervention is important in minimizing the harm. Biochemical markers of recent and high levels of alcohol consumption can play an important role in providing feedback regarding the health consequences of alcohol misuse. Existing markers are not sensitive to recent consumption and in detecting early relapse. Ethyl glucuronide (EtG), a phase-II metabolite of ethanol is a promising marker of recent alcohol use and can be detected in body fluids. In this study an analytical technique for quantitation of EtG in body fluids using solid-phase extraction (SPE) and gas chromatography (GC) with mass spectrometric detection (MS) was developed and validated. Methods: De-proteinization of serum and urine samples was done with perchloric acid and hydrochloric acid, respectively. Serum samples were passed through phospholipids removal cartridges for further clean up. EtG was isolated using amino propyl solid phase extraction columns. Chromatographic separation was achieved by gas chromatography with mass spectrometry. Results: Limit of detection and limit of quantitation were 50 and 150 ng/ml for urine and 80 and 210 ng/ml for serum, respectively. Signal to noise ratio was 3:1, mean absolute recovery was 80-85 per cent. Significant correlation was obtained between breath alcohol and serum EtG levels (r=0.853) and urine EtG and time since last abuse (r = -0.903) in clinical samples. Interpretation & conclusions: In the absence of other standardized techniques to quantitate EtG in biological samples, this gc -ms method was found to have high throughput and was sensitive and specific.

Calificación de un cromatógrafo de gases Agilent Technologies 7890A utilizado en la industria biotecnológica / Qualification of an Agilent Technologies 7890A gas chromatograph used in the biotechnology industry

INTRODUCCIÓN: la producción de medicamentos se rige por estrictas normas internacionales que garantizan la reproducibilidad y consistencia de los resultados obtenidos. La calificación de los instrumentos utilizados en los procesos productivos, así como en la caracterización de los productos y su control de calidad, constituye un requisito previo a la validación de cualquier técnica analítica que haga uso de estos. Una de las técnicas instrumentales utilizada en la industria biotecnológica es la cromatografía de gases. OBJETIVO: desarrollar y ejecutar un protocolo que permita la calificación de un cromatógrafo de gases Agilent Technologies 7890A. MÉTODOS: se empleó un patrón de cafeína pura para análisis y se utilizó una columna HP-5 de 30 m x 0,32 mm d.i. y 0,33 µm espesor de película, en un cromatógrafo de gases acoplado a un detector de ionización de llama. Los diferentes módulos involucrados en el análisis (inyector, columna, horno y detector) se evaluaron a través de un diseño experimental que calcula varios parámetros. RESULTADOS: se obtuvieron pruebas documentadas que demuestran que cada uno de los parámetros estudiados (linealidad del inyector, precisión del inyector, arrastre del inyector, precisión del flujo, exactitud del flujo, linealidad del detector, exactitud del detector, ruido del detector, deriva del detector) cumple con los criterios de aceptación establecidos. CONCLUSIONES: el protocolo desarrollado permite la calificación de un cromatógrafo de gases Agilent Technologies 7890A y puede ser extrapolado a otros modelos(AU)

INTRODUCTION: the drug manufacture is governed by strict international standards that guarantee reproducibility and consistency of results. The qualification of the instruments used in the productive processes, as well as in the characterization of products and their quality control are prerequisites to the validation of any analytical technique using them. One of the instrumental techniques used in the biotechnical industry is Gas Chromatography. OBJECTIVE: to develop and to perform a protocol that allows the qualification of an Agilent Technologies 7890A Gas Chromatograph. METHODS: a standard of pure caffeine was used for analysis in addition to a HP-5 30 m x 0,32 mm d.i. and 0,33 µm thick film column was used in a Gas Chromatograph coupled with a Flame Ionization Detector. For the testing of the different modules involved in the analysis (injector, column, oven and detector), an experimental design was made to estimate several parameters. RESULTS: the obtained documented tests proved that each of the studied parameters (injector linearity, injector precision, injector dragging, flow precision, flow accuracy, detector linearity, detector accuracy, detector noise and detector drift) met the set acceptance criteria. CONCLUSIONS: the final protocol allows the qualification of an Agilent Technologies 7890A Gas Chromatograph and it can be extrapolated to other models(AU)

Analysis of Organophosphate Esters in Dust, Soil and Sediment Samples Using Gas Chromatography Coupled with Mass Spectrometry / 分析化学

Background contamination is a major problem in the analysis of organophosphate esters (OPEs). In this study, the possible sources of OPEs pollution were screened and several different ways were applied to minimize the blank contamination. Under the strict quality control measures, the cleanup efficiency of different solid phase extraction (SPE) was investigated for OPEs in different environmental matrices. A method was developed for the detection of 7 OPEs in dust, soil and sediment samples by gas chromatograph coupled with mass spectrometry ( GC / MS). Target compounds were extracted by hexane:dichloromethane (1 : 1, V/ V) followed by aminopropyl silica gel SPE column cleanup for dust, and target compounds in soil and sediment were Soxhlet extracted and cleanuped by two-step SPE. The results showed that the aminopropyl silica gel SPE column displayed the best purification performance among the three employed columns. Instrumental detection limits among the 7 OPEs ranged from 2. 5 to 25. 8 μg / L, and the method limits of quantification (MLOQs) in dust and soil sample ranged from 1. 4 to 15. 7 ng / g and 0. 3 to 2. 9 ng / g, respectively. The average recoveries of 7 OPEs in different matrices ( dust and soil) at two spiked concentration levels ranged from 67. 9% to 117. 4% . The proposed method was successfully applied to detect OPEs in different environmental matrices collected in Shanghai.

Aplicacao da tecnica por cromatografia a gas para investigacao da formacao de sub produtos da desinfeccao em agua potavel / Application of gas chromatographic technique for investigation of the formation of by products in drinking water disinfection

O uso do cloro para a desinfecção e/ou oxidação nas estações de tratamento de água favorece a formação de subprodutos orgânicos halogenados (SOH), muitos deles carcinogênicos. O objetivo desta pesquisa foi validar uma metodologia analítica proposta para a quantificação simultânea de 12 subprodutos da desinfecção por cromatografia a gás com detector de captura de elétrons (CG-DCE). O método apresentou linearidade (r>0,998), repetibilidade menor que 0,15%, limites de detecção de 1 a 6 µg.L-1 e de quantificação de 3 a 21 Î1/4g.L-1, precisão (<10%), exatidão (93-120%) e recuperação (87-117%). Os resultados indicam que o método pode ser empregado para a investigação de SOH em água, garantindo confiabilidade analítica nos resultados.

The use of chlorine for disinfection and/or oxidation at drinking water treatment plants favors the formation of halogenated organic by-products (HOB), many of them carcinogenic. The purpose of this research was to validate an analytical method for the simultaneous quantification of 12 HOB from disinfection by gas chromatograph with electrons capture detector (GC-ECD). The method provided linearity (r>0.998), repeatability lower than 0.15%, limits of detection from 1 to 6 Î1/4g.L-1 and of quantification from 3 to 21 Î1/4g.L-1, precision (<10%), accuracy (93-120%) and recovery (87-117%). The results indicate that the method can be employed to investigate the formation of HOB in water, yielding analytically reliable results.

Influences of Various Extraction Methods on Content and ChemicalComponents of Volatile Oil from Lignum Santali / 广州中医药大学学报

Objective To observe the influences of ether soaking method, solven t refluxing method and steam distilling method on the content and chemical compo nents of volatile oil from Lignum Santali. Methods Gas chromatograph_mass sp ectrogram (GC_MS) analysis was adopted. Results The content of santalol in t he oi l from Lignum Santali extracted by ether soaking was a little higher than that i n the volatile oil extracted by steam distilling, and their chemical components are similar. The total content of volatile oil extracted by solvent refluxing me thod was 3.35%, much higher than that by steam distilling metho d. GC_MS analysis showed the content of santalol and other chemical components a re similar by the two methods. Conclusion Ether soaking method can be used f or the qualitative analysis of volatile oil from Lignum Santali. Extraction of s antalum oil by steam distilling method is incomplete.

Determination of Organic Chloride Pesticides and Polycyclic Aromatic Hydrocarbons in Prophyra by Gas Chromatograph-Mass Spectrometry / 环境与健康杂志

Objective To develop an analytical method by gas chromatograph-mass spectrometry(GC-MS) for the determination of organic chloride pesticides and polycyclic aromatic hydrocarbons in prophyra Methods The samples were extracted by an acetone-hexane(7∶3,V/V) mixture first,then were purified by C18 solid-phase extraction(SPE),and then were determined with GC-MS.Results The linear range was 0.01-5.0 ?g/ml,the limits of detection were 0.05-0.32 ng/g(dry weight) and 0.25-0.56 ng/g(dry weight)for organic chloride pesticides and polycyclic aromatic hydrocarbons respectively.The recovery rates and relative standard deviation for organic chloride pesticides were 74.27%-121.49% and 3.19 %-17.31% relatively;the recovery rates and relative standard deviation for polycyclic aromatic hydrocarbons were 65.10%-119.26% and 2.75%-14.11% relatively.Organic chloride pesticides were partly detected,but the detection rate of polycyclic aromatic hydrocarbons was higher.Fifteen polycyclic aromatic hydrocarbons were detected in all samples but dibenz(a,h)-anthracene.Conclusion This method is sensitive,accurate and applicable to the determination of organic chloride pesticides and polycyclic aromatic hydrocarbons in prophyra.

DETERMINATION OF FREE RESVERATROL IN GRAPE WINE BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY / 营养学报

Objective: In this paper, a method of gas chromatography mass spectrometry for determination of free resveratrol in grape wine was established. Methods: After evaporated to eliminate ethanol, sample of grape wine was extracted with ethyl acetate, and evaporated again to dryness. The residues were derivatized with N,O bis (trimethylsianyl) trifluoroacetamide plus 1% trimethychlorosilane. Then, qualitative and quantitative analysis of cis and trans resveratrol were carried out using GC MS scan mode. Results: The average recoveries were 85.6%-110.5%,and the relative standard deviations were 8.2%-11.5%, when resveratrol was added to grape wine at 0.25-1.25 mg/L levels. The correlation coefficient was 0.995 in range of 0.50-10.00 mg/L. The detection limit for resveratrol in grape wine was 0.005 mg/L. Further 15 grape wines made in China were analyzed. The contents of cis resveratrol were 0.02 -0.56 mg/L and trans resveratrol were 0.15-1.28 mg/L. Total resveratrol were 0.26-1.48 mg/L. Conclusion: This assay is accurate and reproducible for determination of free resveratrol in grape wines.