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A new derivative of ordered mesoporous carbon (GSH-CMK-3) has been prepared by chemical modification and functionalization of ordered mesoporous carbon with glutathione. The composite was fully characterized by means of Fourier transforming infrared spectroscopy (FT-IR), scanning electron microscope (SEM) image and thermogravimetric analysis (TGA). GSH-CMK-3 showed favorable chemical stability, thermal stability and excellent adsorption performance toward Cd2+and a maximum adsorption capacity of 87.87 mg/g was achieved. The adsorption kinetic follows pseudo-second-order adsorption model. In a sequential injection mini-column separation system, 0. 006 mol/L sulfourea (in 0. 2 mol/L HNO3) was adopted as eluent and the elution efficiency was 96%. With a sample volume of 1000 μL and 50 μL of eluate, an enrichment factor of 17.3 was obtained. A procedure for on-line selective separation and preconcentration of trace Cd2+was developed by graphite furnace atomic absorption spectrometry. Along with a detection limit of 1.9 ng/L (n=7,3σ) and a linear range of 0.05-0.20 μg/L, a RSD of 2.9% (n=13,100 ng/L) was achieved. The method was validated by analyzing Cd2+in a certified reference material GBW08608.
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OBJECTIVE: To establish a method for determining arsenic (As) and antimony (Sb) released from pharmaceutical glass packing materials to provide reference for improving the existing quality standard. METHODS: The samples were filled with 4% acetic acid to leach As and Sb. The extracting temperature was 98℃, and the extracting time was 2 h. Graphite furnace atomic absorption spectrometry (GFAAS) was used for the determination. RESULTS: As and Sb showed good linear relationship in a certain concentration range with linear correlation coefficients of 0.999 9 and 0.999 5. The recovery rates were 94.7%-106.9% and 100.0%-106.3%. The relative standard deviations of precision were 2.3% and 2.9%. The relative standard deviations of repeatability were 6.5% and 6.9%. The limits of detection were 1.67 and 2.54 ng·mL-1, respectively. The elements were nearly not detected in 16 batches of samples. CONCLUSION: The method is efficient and accurate and can be used for determination of As and Sb released from pharmaceutical glass packing materials, which brings supplementary contents to the existing quality standard.
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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 investigate the lead and cadmium contents in different sampling sites from full term neonatal placenta and to explore the role of placental sample in the evaluation of intrauterine heavy metals exposure.Methods The placentas from 30 healthy full term neonates were collected from the West China Second Hospital of Sichuan University during May and June 2016.Each placenta fetal side was divided into the left and right parts with the umbilical vein in the umbilical cord cross-section as the 12 o'clock direction.The villus lobular tissue samples were taken from the 1/4 radius in left part (site A) and 3/4 radius in the right part (site B).The graphite furnace atomic absorption spectrometry was used to detect the lead and cadmium contents in the samples.The elements contents in the site A and B were performed the paired t-test and correlation analysis.Results The mean contents of lead and cadmium in dry weight sample at placental site A were 91.8 and 66.7μg/kg which at the site B were 88.9 and 64.8 μg/kg respectively.The lead and cadmium contents at these two sites presented the positive correlation,the coefficients were 0.98 and 0.97 respectively,whereas the difference in contents between the tissues from different placental sites had no statistical significance.Conclusion The lead and cadmium contents of villus lobular tissue in the central part of placenta fetal side (1/4-3/4 radius area) are basically consistent,which is a reliable indicator for evaluating the intrauterine heavy metals exposure.
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OBJECTIVE: To establish a methodology to dilute blood sample with compound matrix modifier,and to determine the blood level of nickel using improved graphite furnace atomic absorption spectrometry( GFAAS). METHODS: The blood samples( 100. 00 μL) were diluted 5 times in 0. 12 g / L mass concentration of palladium chloride combined with 1. 00 %(V /V) Triton X-100 and 0. 10%(V /V) nitric acid,and the blood level of nickel was detected by GFAAS. RESULTS: The good linearity range of nickel mass concentration in blood was 0. 30-25. 00 μg / L,the correlation coefficient was 0. 999 7,the detection limit was 0. 30 μg / L,the minimum detectable mass concentration was 1. 50 μg / L,the recovery rate was99. 00 %-102. 75 %. The within-run and between-run relative standard deviations were 1. 43 %-3. 70 % and 2. 20 %-5. 03 %,respectively. Blood samples can be stored for at least 7 days at 4 ℃. CONCLUSION: This method is simple for operation,with high accuracy and precision,which is suitable for determination of nickel in blood in normal individuals and workers with occupational exposed to nickel.
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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 establish a method for determination of trace platinum in zolpidem tartrate. METHODS:Graphite furnace atomic absorption spectrometry(GFAAS)was adopted for direct determination after dissolving sample in 1% Hydrochloric acid solution. Horizontal platform graphite tube was performed with detection wavelength of 244.79 nm,slit width of 0.2 nm and current intensity of hollow cathode lamp of 6 mA. The mode of background correction was zeeman effect,the peak height was used as measurement pattern,and the injection volume was 20 μl. RESULTS:The linear range of platinum was 0-100 ng/ml(r=0.999 0);RSDs of precision and reproducibility tests were no more than 2.0%;recovery was 97.78%-103.07%(RSD=1.6%,n=9);the detection limit was 1.48 ng/ml. CONCLUSIONS:This method is simple and rapid with good precision and accuracy,and can be applied for the determination of trace platinum in zolpidem tartrate.
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OBJECTIVE:To establish the methods for content determination of lead and cadmium in Achyranthes bidentata from different habitats.METHODS:Graphite furnace atomic absorption spectrometry was applied.RESULTS:There were a good linear relationship between the concentration and absorbance of lead and cadmium.The linear range of lead were 0～80.00 ?g?L-1(r=0.999 6) with recovery of 95%～101%(RSD ranged from 0% to 5.00%,n=10).The linear range of cadmium were 0～7.000 ?g?L-1(r=0.998 2) with recovery of 98%～103%(RSD ranged from 1.00% to 5.00%,n=10).CONCLUSION:The method is simple,accurate,convenient and sensitive and the results are satisfactory.
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Objective To select a matrix modifier,which can effectively eliminate the matrix interference in the determination of chromium in cosmetics by graphite furnace atomic absorption spectrometry(GFAAS).Methods The orthogonal experiment design was used to define the best operation parameter of graphite furnace.Vitamin C,(NH4)H2PO4,(NH4)2HPO4,NH4Cl and Mg(NO3)2 were added respectively as the matrix modifiers.The effect of five matrix modifiers was compared by precision test.Results When(NH4)H2PO4 was taken as the chemical modifier,the determination result was satisfied.The characteristic mass was 5.68?10-12 g,relative standard deviation were from 2.11% to 4.46%.The rate of recovery of two cosmetics samples were 95.2% and 102.01%.Conclusion(NH4)H2PO4 can increase the ashing temperature,decrease the atomization temperature,eliminate the matrix interference and the result has good precision and accuracy.
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Objective To develop a method to determine lead in the whole blood with graphite furnace atomic absorption spectrometry.Methods The whole blood was diluted with mixing matix modifiers [5.0 g/L NH4H2PO4+1.0 g/L Tritonx-100+2.0 ml/L HNO3],then the samples were automatically injected and the blood lead level was determined with Zeeman graphite furnace atomic absorption spectrometer.Results There was significant linear relation between absorbance and lead level in the range of 0-40 ?g/L(r=0.998 2),the relative standard deviation(RSD)was 5.5%-12.2%,the recovery rate was 90%-106%,detection limit was 1.1 ?g/L.Conclusion This method is characterized by reliable result,convenient procedure as well as lower pollution.The test result of whole blood lead level in more than 600 occupational lead exposed people with this method is satisfactory.
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ve To develope a new graphite furnace atomic absorption spectrophotometric (GFAAS) method for determination of cobalt in cosmetics. Methods Samples were digested by HNO3-HCl and microwave. The use of a new matrix modifier, (NH4)2 HPO4-ascorbic acid as a matrix, could effectively improve the shape of peak and eliminate the matrix interferences.The best determination conditions, such as the procedure of sample digestion, the measurement parameters were defined in this assay. Results The characteristic concentration, linear range, re-covery rate and coefficient of variation were 1.2?g/L, 0 -40?g/L, 100.16% ~102.01% and 1.82%-3.26% re-spectively. Conclusion Application of matrix modifier (NH4)2 HPO4-ascorbic acid for determination of Co with GFAAS, was easy and presented good repeatibility.