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OBJECTIVE: To improve the pretreatment method for the detection of lead, manganese and their inorganic compounds in workplace air samples by flame atomic absorption spectrometry. METHODS: In this method, 20.0 mL of 1.0-2.0 mol/L nitric acid solution was used as the digestion solution to digest the microporous membrane sample at 140-160 ℃ to a volume of 0.5-1.0 mL. Samples were cooled and fixed to 10 mL and detected by flame atomic absorption spectrometry method. RESULTS: The lead detection had a good linear relationship in the range of 0.10-3.00 mg/L. The correlation coefficient was 0.999 5, the detection limit and the lower limit of quantification were 0.03 and 0.10 mg/L respectively(calculated by 3 and 10 times of standard deviation respectively). The minimum detection concentration was 0.004 mg/m~3, and the minimum quantitative concentration was 0.010 mg/m~3(collected by 75 L air calculation). The manganese detection had a good linear relationship in the range of 0.05-3.00 mg/L mass concentration. The correlation coefficient was 0.999 8, the detection limit and the lower limit of quantification were 0.015 and 0.05 mg/L respectively(calculated by 3 and 10 times of standard deviation respectively), the minimum detection concentration was 0.002 mg/m~3, and the minimum quantitative concentration was 0.007 mg/m~3(based on collection 75 L air calculation). The recovery rate of standard addition was 97.8%-99.6%, and the relative standard deviation within and between run were 0.4%-2.0% and 0.4%-1.7% respectively. CONCLUSION: The method is simple, the reagent consumption is small, the digestion temperature is low, the precision and accuracy are high. This method is suitable for widespread use.
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This study focuses on the heavy metals concentrations (Fe, Cu, Zn, Pb, and Cd) in certain common milk species are collected from Iraqi markets using Flame Atomic Absorption Spectrophotometer-6300 AA, Shimadzu, Japan, respectively. This study shows the pollution in the environment obtained by heavy metals. The results showed that Cr, Cd, Cu, Zn, and Fe were varying according to the order: Zn>Fe>Cr>Cd>Cu. levels of heavy metals were 0.610(Cr), 0.125(Cd), 0.052(Cu), and 6.902(Zn), and 0.759(Fe). All the heavy metals were observed within maximum limit in milk. Overall, the number of analyzed heavy metals and sample size were limited in present study. Keywords: Heavy metals; Milk; Najaf; Flame atomic absorption; Spectrophotometer This study focuses on the heavy metals concentrations (Fe, Cu, Zn, Pb, and Cd) in certain common milk species are collected from Iraqi markets using Flame Atomic Absorption Spectrophotometer-6300 AA, Shimadzu, Japan, respectively. This study shows the pollution in the environment obtained by heavy metals. The results showed that Cr, Cd, Cu, Zn, and Fe were varying according to the order: Zn>Fe>Cr>Cd>Cu. levels of heavy metals were 0.610(Cr), 0.125(Cd), 0.052(Cu), and 6.902(Zn), and 0.759(Fe). All the heavy metals were observed within maximum limit in milk. Overall, the number of analyzed heavy metals and sample size were limited in present study
Subject(s)
Spectrophotometry, Atomic , Flame Spectrophotometers , Metals, Heavy/toxicity , MilkABSTRACT
Background: The gross composition of human milk is remarkably constant among women of varying nutritional status. Reliable information is now available on the content, and the principal factor affecting it, of most of the trace elements on human milk. However, for some of the trace elements, there is still a wide variation in reported values in the literature, which is due at least in part, to analytical difficulties. Hence this study was taken up to find out if maternal nutritional status influences the copper and zinc concentrations in colostrum of mother.Methods: Total of 100 mothers were enrolled in the study after obtaining prior informed consent. They were divided into 2 groups - group I had 50 malnourished mothers and group II had 50 well-nourished mothers. Sample digestion was attempted with different quantities of various acids. Analysis of digested colostrum was carried out for copper and zinc.Results: The mean levels of copper and zinc were slightly more among well-nourished than malnourished women. Values of copper were significantly higher in the colostrum of well-nourished as compared to that of the malnourished mothers.Conclusions: The parameters of weight, height weight/height ratio and hemoglobin varied significantly between the well-nourished and malnourished mothers. The difference in milk content of malnourished and well-nourished mothers is not significant for zinc. However, copper levels were significantly higher in well-nourished mothers.
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Background: Minerals and trace element content of human milk have been a matter of concern among nutritionist in relation to the availability of the essential elements to the new born. Mineral and trace elements occur in the body in a number of chemical forms, such as inorganic ions and salts, or as constituents of organic molecules, for example proteins, fats, carbohydrates and nucleic acids. There is a paucity of data on the effect of nutrition on the composition of trace elements in milk and its effect on the infant. Hence a comparison made between the trace element and mineral such as sodium, potassium, magnesium, iron, zinc, copper, calcium in milk of malnourished and well-nourished mothers in order to determine the effect of maternal nutrition on the quality of milk and its effect on the growth and physical development of the new-born.Methods: Around 100 mothers were enrolled in the study after obtaining prior informed consent. They were divided into 2 groups-group I had 50 malnourished mothers and group II had 50 well-nourished mothers. The pre-fed milk sample which was collected was stored at - 20℃ until it was processed. It was thawed and analysed for copper, zinc, iron, magnesium, sodium, potassium and calcium.Results: The mean levels of trace elements (iron and zinc) and minerals (sodium, potassium, calcium, magnesium) were slightly more among well-nourished than malnourished women. Values of only copper were significantly higher in the colostrum of well-nourished as compared to that of the malnourished mothers.Conclusions: The parameters of weight, height weight/height ratio and hemoglobin varied significantly between the well-nourished and malnourished mothers. The difference in milk content of malnourished and well-nourished mothers is not significant for sodium, potassium, calcium, iron, magnesium, zinc. However, copper levels were significantly higher in well-nourished mothers.
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Abstract A 32 factorial design was employed to develop an in vitro digestion method for estimation of Fe bioaccessible fractions in cooked chicken meat. The effects of sample size and the in vitro bioaccessible fractions of this essential element were evaluated. A sample preparation method employing a microwave assisted digestion with dilute nitric acid was used prior to total Fe determination. For the bioacessibility studies, the optimized procedure employed 7.5 g of sample and 6% w/v of an acid pepsin solution. This procedure was applied to two kinds of chicken meat samples: breast and liver. Flame Atomic Absorption Spectrometry was used to determine total and bioaccessible (chyme or soluble portion) levels of iron in the samples. With respect to total Fe content, the bioaccessible fractions of Fe found in these samples were around 23% and 56 %, for breast and chicken liver, respectively. The chicken liver sample showed the highest total (400 ± 10 mg kg-1) and bioaccessible Fe contents (223 ± 18 mg kg-1) and stands out as a good source of this micronutrient.
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OBJECTIVE:To establish a method for the contents determination of 5 heavy metals in Ershiwuwei shanhu pills, and to investigate the contents of heavy metals in Ershiwuwei shanhu pills produced by 5 manufacturers from different districts of Tibet. METHODS:Ershiwuwei shanhu pills were digested by HNO3-HClO4(4:1,V/V).The contents of 3 heavy metals as Cu,Pb, Cd in samples were measured by flame atomic absorption spectrometry(FAAS). The contents of 2 heavy metals as As,Hg in samples were measured by hydride generation atomic absorption spectrometry(HG-AAS). RESULTS:5 kinds of heavy metals have good linear relationship in the corresponding mass concentration range(all r≥0.999 1). The limits of detection of Cu,Pb, Cd were 0.001 6,0.041 2,0.036 3 mg/L,and the limits of quantitation were 0.005 3,0.137 3,0.121 0 mg/L;the limits of detection of As,Hg were 0.325 7,0.692 3 μg/L,and the limits of quantitation were 1.085 7,2.307 7 μg/L. RSDs of precision tests were ≤5.54%(n=6);RSDs of stability tests were all≤3.79%;RSDs of reproducibility tests were ≤3.72%. The average recovery rates were 91.34%-110.11%(RSDs were 0.66%-6.80%,n=6). Results of contents determination showed that the contents of Cu in samples from 5 manufacturers were not out of limits,but the contents of Cd and Hg were all out of limits; the contents of Pb in samples from 4 manufacturers were out of limits,and the contents of As in samples from 2 manufacturers were out of limits. CONCLUSIONS:The established method has good accuracy,sensitivity,stability and reproducibility,and it is suitable for contents determination of 5 heavy metals in Ershiwuwei shanhu pills. To some extent,there is a problem of excessive heavy metals in samples from 5 manufacturers.
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OBJECTIVE:To provide reference for improving the quality of Gelatin hollow capsule. METHODS:Atomic fluo-rescence spectrometry was used to determine the contents of Hg,As in Gelatin hollow capsule;graphite furnace atomic absorption spectrometry was used to determine the contents of Cr,Pb,Cd;flame atomic absorption spectrometry was used to determine the contents of Cu,Zn;and the contents of 7 elements in 48 batches of commercially available Gelatin hollow capsule were deter-mined. RESULTS:Each element showed good linear relationship in each mass concentration range(Cr,Pb,Cd,As and Hg were respectively 0-10,0-20,0-1.5,0-10,0-1.0μg/L;Cu and Zn were 0-1.8 mg/L)(r≥0.9969). The detection limits of Cr,Pb,Cd, Cu,Zn,Hg and As were 0.065,0.007,0.011,0.004,0.010,0.108,0.004 μg/L,respectively. RSDs of precision tests were no more than 2.5%(n=6);RSDs of reproducibility tests were no more than 7.5%(n=6);average recoveries ranged in 88.6%-109.5%(RSD≤6.7%,n=6). The contents of 7 elements in the 48 batches of samples were in line with the relevant provi-sions in Chinese Pharmacopoeia(2015 edition,part 4)and pharmacopoeia or standards in other countries or organizations. CON-CLUSIONS:The method shows high sensitivity,high precision with accurate and reliable results,and can be used for the content determination of Cr,Pb,Cd,Cu,Zn,Hg and As in Gelatin hollow capsule. The 48 batches of Gelatin hollow capsule from differ-ent manufacturers have good quality.
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OBJECTIVE:To provide reference for improving the quality of Gelatin hollow capsule. METHODS:Atomic fluo-rescence spectrometry was used to determine the contents of Hg,As in Gelatin hollow capsule;graphite furnace atomic absorption spectrometry was used to determine the contents of Cr,Pb,Cd;flame atomic absorption spectrometry was used to determine the contents of Cu,Zn;and the contents of 7 elements in 48 batches of commercially available Gelatin hollow capsule were deter-mined. RESULTS:Each element showed good linear relationship in each mass concentration range(Cr,Pb,Cd,As and Hg were respectively 0-10,0-20,0-1.5,0-10,0-1.0μg/L;Cu and Zn were 0-1.8 mg/L)(r≥0.9969). The detection limits of Cr,Pb,Cd, Cu,Zn,Hg and As were 0.065,0.007,0.011,0.004,0.010,0.108,0.004 μg/L,respectively. RSDs of precision tests were no more than 2.5%(n=6);RSDs of reproducibility tests were no more than 7.5%(n=6);average recoveries ranged in 88.6%-109.5%(RSD≤6.7%,n=6). The contents of 7 elements in the 48 batches of samples were in line with the relevant provi-sions in Chinese Pharmacopoeia(2015 edition,part 4)and pharmacopoeia or standards in other countries or organizations. CON-CLUSIONS:The method shows high sensitivity,high precision with accurate and reliable results,and can be used for the content determination of Cr,Pb,Cd,Cu,Zn,Hg and As in Gelatin hollow capsule. The 48 batches of Gelatin hollow capsule from differ-ent manufacturers have good quality.
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OBJECTIVE:To study the extraction rate and speciation of antivitiligo-related elements in Opercalina turperthum by water extraction and semi-bionic extraction. METHODS:Water extraction and semi-bionic extraction were respectively used. Wa-ter-soluble state and suspension state in extract of O. turperthum were separated by microporous filtering film;organic and inorgan-ic trace elements in water-soluble state were separated by macroporous resin. The contents of Cu,Zn,Fe,Ca,Mg,Mn and Sr were detected by flame atomic adsorption spectrophotometry,and speciation analysis was conducted. RESULTS:After water extrac-tion,extraction rates of 7 trace elements were 40.47%-72.49%;ratio of suspended particles was 3.69%-8.78%;ratio of organic state/inorganic state was 104.36% in water-soluble state of Sr and 3.94%-48.39% in water-soluble state of Cu,Zn,Fe,Ca,Mg, Mn. After semi-bionic extraction,except for Mn,extraction rates of trace elements were higher than water extraction,extraction rates of Cu,Zn,Fe,Ca,Mg,Sr were 77.69%-90.19%;ratio of suspended particles was 0.39%-8.57%;the ratio of organic state/inorganic state was 72.74%-180.79% in water-soluble state of elements. CONCLUSIONS:Cu,Zn,Fe,Ca,Mg,Mn and Sr in O. turperthum are dissolved easily,mainly existing in the form of inorganic state. After semi-bionic extraction,except for Mn,the dis-solution rate of other elements and the proportion of organic trace elements after dissolution increase significantly. Both dissolution and effective utilization rate of trace elements by semi-bionic extraction are higher than water extraction.
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OBJECTIVE:To establish a method for the contents determination of microelements in Chrysanthemum indicum from different production fields. METHODS:Graphite furnace atomic absorption (GFAAS) was used to determine the contents of Pb,Cd and As;HGAAS was used to determination the content of Hg;and FAAS was used to determine the contents of Cu,Fe, Mn,Ca,Mg and Zn. RESULTS:The linear range was 0-50 μg/L for Pb(r=0.999 9),0-10 μg/L for Cd(r=0.999 2),0-50 μg/L for As(r=0.999 0),0-20 μg/L for Hg(r=0.999 5),0-5 μg/L for Cu(r=0.999 3),0-15 μg/L for Fe(r=0.999 8),0-2 μg/L for Mn (r=0.999 9),0-50 μg/L for Ca(r=1.000 0),0-20 μg/L for Mg(r=0.999 9)and 0-2 μg/L for Zn(r=0.999 8);RSDs of precision, stability and reroducibility tests were lower than 3%;recoveries were 94.25%~97.43%(RSD=1.07%)、94.97%~99.46%(RSD=1.68%)、96.25%~99.46%(RSD=1.09%,n=6)、96.61%~99.91%(RSD=1.26%,n=6)、94.11%~98.41%(RSD=1.68%,n=6)、93.11%~99.59%(RSD=2.73%,n=6)、93.11%~99.48%(RSD=2.63%,n=6)、93.01%~99.85%(RSD=2.49%,n=6)、95.13%~99.75%(RSD=1.58%,n=6)、94.08%~97.37%(RSD=1.18%,n=6),respectively. CONCLUSIONS:The method is simple,stable and reproducible,and can be used for the contents determination of microelements in C. indicum from different pro-duction fields.
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OBJECTIVE: To improve the standard detection method of tin and its compounds in the air of workplace.METHODS: During the sample preparation,the amount of sulfuric acid for air filter membrane digestion was reduced from its original 0. 5 m L( the standard method of flame atomic absorption spectrometry) to 0. 2 m L and no acid-driving after the membrane was digested. The amount of sulfuric acid given to the series of standards was the same as that of the membrane digestion. The samples were detected by the flame atomic absorption spectrometry method. RESULTS: The improved method showed a good linear range of tin as 0. 0-80. 0 mg / L,the regression equation was
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Objective:To determine the content of copper and zinc in tea by flame atomic absorption spectrophotometry and to investigate the influence on the content after leached for different time. Methods:The tea samples were leached for different time by boiling water and then the content of copper and zinc was determinated by flame atomic absorption spectrophotometry. Results:When the leaching time was less than 10 min, the content of copper and zinc increased significantly with the prolongation of the leaching time, while the increase was not obvious when the leaching time was more than 10 min. Copper and zinc showed good linearity in the range of 0.02-0.15 mg/L and 0.05-0.30 mg/L,separately. The recovery was in the range of 98.5%-101.1%for copper and 98.7%-101.2%for zinc with the RSD of 0.8%in copper and zinc (n=9) . Conclusion:The method is suitable to determine the content of copper and zinc in tea. Leaching time can influence the content of copper and zinc in tea significantly.
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Introduction: The therapeutic monitoring of lithium, through concentration measurements, is important for individual dose adjustment, as a marker of treatment adherence and to prevent poisoning and side effects. Objectives: Validate and compare two methods - atomic emission and atomic absorption - for the determination of lithium in serum samples. Methodology: Parameters such as specificity, precision, accuracy, limit of detection (LOD) and linearity were considered. The atomic absorption spectrometer was used, operating in either emission or absorption mode. For the quantitative comparison of 30 serum samples from patients with mood disorder treated with lithium, the results were submitted to Student's t-test, F-test and Pearson's correlation. Results: The limit of quantification (LOQ) was established as 0.05 mEq/l of lithium, and calibration curves were constructed in the range of 0.05-2 mEq/l of lithium, using aqueous standards. Sample preparation time was reduced, what is important in medical laboratory. Conclusion: Both methods were considered satisfactory, precise and accurate and can be adopted for lithium quantification. In the comparison of quantitative results in lithium-treated patients through statistical tests, no significant differences were observed. Therefore the methods for lithium quantification by flame atomic absorption spectrometry (FAAS) and flame atomic emission spectrometry (FAES) may be considered similar...
Introdução: A monitorização terapêutica por meio da determinação sérica de lítio é importante para proporcionar o ajuste individual da dose, como marcador de adesão e para prevenir intoxicações. Objetivos: Validar e comparar duas metodologias, a de emissão e a de absorção atômicas, para determinação de lítio em amostras de soro. Metodologia: Foram determinados parâmetros de especificidade, precisão, exatidão, limite de detecção e linearidade a fim de validar as metodologias para determinação de lítio. Foi utilizado espectrômetro de absorção atômica, funcionando no modo de emissão ou de absorção. Para comparação das metodologias foram utilizados os testes estatísticos (teste t de Student, o teste F e a correlação de Pearson) nos resultados quantitativos de 30 amostras de soro sanguíneo de pacientes que faziam uso terapêutico de lítio para o controle do transtorno de humor bipolar (THB). Resultados: Foram estabelecidos um limite de quantificação de 0,05 mEq/l de lítio e curvas de calibração de 0,05 a 2 mEq/l de lítio, construídas utilizando padrões aquosos, com redução no tempo de preparo das amostras, principalmente para ser utilizado em laboratório de análises clínicas. Conclusão: Os dois métodos foram considerados satisfatórios, precisos e exatos e podem ser adotados para a quantificação do lítio. Na comparação dos dois métodos por testes estatísticos em amostras de pacientes tratados com o fármaco, não foram observadas diferenças significativas entre os resultados encontrados. Desta forma, os métodos para quantificação do lítio por espectrometria de absorção atômica em chama (FAAS) e espectrometria de emissão atômica em chama (FAES) podem ser considerados semelhantes...
Subject(s)
Humans , Spectrum Analysis/methods , Lithium/analysis , Validation Studies as TopicABSTRACT
This study was aimed to determine trace elements in Peach pulp . The wet digestion method and car-bonize acid dissolution method were applied to digest the sample, and flame atomic absorption spectroscopy was used to determine the content of trace elements (Fe, Cu, Mn) in Peach pulp . The results showed that the content is not consistent among different pretreatment methods. However, the metalion content among these three methods are in the order of Fe > Mn > Cu, with the average recovery rate between 92.6% and 119.6%. The RSD is less than 2.86%. It was concluded that this method is with high accuracy and stability as well as reliable accurate re-sults. It also proved that Peach pulp . is rich in Fe, Cu and Mn. It provides some useful information for further pharmacological study of Peach pulp .
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Objective To study the difference of content of Cu、Fe、Mn、Zn、Cr in urine between electroplating industry personnel and health population. Methods Flame atomic absorption spectrometry (FAAS) was used to determine the levels of Cu、Fe、Mn、Zn、Cr in the samples both of fresh urine and the urine treated by nitric acid and perchloric acid. The data was analyzed by SPSS software. Results Among 380 objects (190 industry personnel, 190 health persons), elentroplating industry personnel had significantly higher Zinc level (P < 0.01). Other trace elements levles were not significantly different between the two groups. Conclusion FAAS was a simple, rapid and stable method, with low relative error, 2.22%～4.02% of RSD and 95.2%～106.0% of recovery rate. It were found that some occupational hazards exist.
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Objective To determine the total sodium in Danshen for injection.Methods Flame atomic absorption spectroscopy was used to determine the total sodium in Danshen for injection.Results The calibration curves were linear in the range of 0.5～10 mg/L for sodium chloride.The average recovery rates of sodium chloride were 101.8%,RSD=1.60%.Conclusion This method was found to be simple,quick and accurate for simultaneous determination of sodium in Danshen for injection.
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Objective To determine the contents of elements Fe, Mn, Ni, Cu, Zn, Ca, Mg and Cr in Gentiana macrophlla and Gentiana officinalis. Methods The contents of elements were determined by flame atomic absorption spectrometry. Results The recovery rates obtained by standard addition method were between 88.1%～114.5%, and the RSDs were lower than 3.18%. Gentiana macrophlla is rich in the trace elements such as Fe, Ni, Cu, Ca, Mg, and Gentiana officinalis is rich in the trace elements such as Mn, Zn, Cr. Conclusion There are some difference between wild and planted Gentiana officinalis in element content, that may be related to their growing environment.
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0.05). Conclusion The extract technology is basically reasonable,and need further improvement.
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Objective To develop a new method for the determination of trace silver in water by flame atomic absorption(FAAS) after cloud point extraction.Methods Diethyldithiophosphate(DDTP) and triton X-114 were respectively used as the chelating agent and surfactant.The effects of experimental conditions such as acidity,concentration of chelating agent,surfactant and methanol,equilibration temperature and time,interference ion on cloud point extraction were investigated.Results Under the optimum condition,0.5 ml of 0.1 mol/L DDTP solution,0.5 ml of 50 g/L Triton X-114 and 5 ml of 1 mol/L hydrochloric acid were added and the volume was made up to 50 ml.The mixture was heated in a thermostatic bath at 40 ℃ for 15 min,the linear range of determination for silver was 0-100 ng/ml,the equation of linear regression was A = 0.005 8cAg+ 0.001 6,r = 0.999.The detection limit was 0.83 ng/ml,the recovery rate was in the range of 97%-105%,and the relative standard deviation was 3.1%(n=11) for 20 ng/ml Ag.There was no significant interference for silver solution containing 5 000 times of K+,Na+,Ca2,Mg2,NO3,SO4 + +-2-and Cl-,1 000 times of Al3+ and Zn2+,500 times of Fe2+ and Mn2+,100 times of Pb2+ and Cu2+.Conclusion The method is rapid,accurate,simple and applicable to the determination of trace silver in water samples.
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Objective To develop a new method for the determination of trace manganese in water by flame atomic absorption after cloud point extraction. Methods The effect of experimental conditions such as pH value and concentration of reagents and equilibration temperature on cloud point extraction and determination sensitivity was discussed. The chemical variables affecting the separation phase and extraction recovery were optimized. Results Under the optimum conditions, pre-concentration of only 50 ml of sample in the presence of 0.05% Triton X-114 presented a detection limit of 0.28 ?g/L(3?) for manganese. The enhancement factor was 65 for manganese. The relative standard deviation was 2.17%. The calibration graph using the pre-concentration system for manganese was linear with a correlation coefficient of 0.999 at levels near the detection limits up to at least 120 ?g/L. The recovery rates were 98.0%-101.5%. Conclusion The method is rapid, accurate, simple and is suitable for determination of trace manganese in water samples.