IImprovement of pretreatment method for detection of lead, manganese and their inorganic compounds in the air of workplace by flame atomic absorption spectrometry / 中国职业医学

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.

Multivariate approach to assess in vitro Fe bioaccessibility in chicken meat

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.

Contents Determination of 5 Heavy Metals in Tibetan Medicine Ershiwuwei Shanhu Pills by Atomic Absorption Spectrometry / 中国药房

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.

Establishment and Application of Content Determination Method for 7 Elements in Gelatin Hollow Capsule / 中国药房

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.

Establishment and Application of Content Determination Method for 7 Elements in Gelatin Hollow Capsule / 中国药房

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.

Improving the detection method for tin and its compounds in workplace air / 中国职业医学

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

Contents Determination of Microelements in Chrysanthemum indicum from Different Production Fields / 中国药房

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.

Determinação sérica de lítio: comparação das metodologias de espectrometria de emissão e de absorção atômica / Determination of serum lithium: comparison between atomic emission and absorption spectrometry methods

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...

Determination of Trace Elements in Urine of Electroplating Industry Personnel in Longwan District of Wenzhou City with Flame Atomic Absorption Spectrometry / 预防医学

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.

Determination of the Content and Dissolution Rate of Trace Elements in Antivirus Formula and Its Extract / 中药新药与临床药理

0.05). Conclusion The extract technology is basically reasonable,and need further improvement.

Determination of Trace Silver in Water Samples by Flame Atomic Absorption Spectrometry after Cloud Point Extraction / 环境与健康杂志

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.

Determination of Trace Manganese in Water Samples by Flame Atomic Absorption Spectrometry with Cloud Point Extraction / 环境与健康杂志

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.