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ObjectiveTo obtain content characteristics of inorganic elements in Scutellariae Radix （aged 1-4 years）， and to explore the feasibility of identifying the growth years of Scutellariae Radix based on characteristic spectrum of inorganic elements combined with chemometric models. MethodAfter microwave digestion， the contents of Mn， Zn， Ca， Fe， Mg， Na， K， Cr， Cu， Se， As， Cd， Hg， Pb and Ni in 21 batches of Scutellariae Radix were determined by inductively coupled plasma atomic emission spectrometry （ICP-OES） and inductively coupled plasma mass spectrometry （ICP-MS）. Meanwhile， characteristic spectrum of inorganic elements in samples was drawn. The identification model was constructed to discriminate the growth years of Scutellariae Radix based on the combination of principal component analysis （PCA）， Fisher discriminant function and support vector machine （SVM）. ResultThe contents of Mn （7.79-36.48 μg·g-1）， Zn （10.12-31.43 μg·g-1）， Cu （6.38-17.20 μg·g-1）， K （2.98-13.89 μg·g-1）， Mg （3.45-7.78 μg·g-1） and Ca （2.32-7.09 μg·g-1） in Scutellariae Radix were detected by ICP-OES and ICP-MS， and their contents increased with the prolongation of growth years. PCA results showed that Cu， Ni， Cd， Na， Mg， Fe， Ca， Zn， Mn and Hg were characteristic elements of Scutellariae Radix. Samples with different years could be divided into four categories in the spatial characteristic diagram of Fisher discriminant analysis. The correct rate of SVM model for identifying the growth years of samples was 95.2%. ConclusionThis established method is accurate and rapid for discriminating the growth years of Scutellariae Radix， which can provide reference for the identification of other Chinese medicinal materials. It is suggested that some elements should be considered as indexes in subsequent construction of the quality evaluation system of Scutellariae Radix.
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Objective:To analyze and determine heavy metal content in Paridis Rhizoma from different genus and localities,in order to provide a reference for selecting cultivation areas and establishing the quality standard of Paridis Rhizoma of heavy metals content. Method:Microwave digestion method combined with inductively coupled plasma atomic emission spectrometry method (ICP-AES) method were applied to determine the contents of 6 heavy metals,i.e. As,Cu,Hg,Cd,Pb and Cr in 39 samples of Paridis Rhizoma of different genus and localities in Yunnan Province. Cluster analysis,statistical analysis and principal component analysis (PCA) were used to compare the differences of heavy metals contents in different localities and species. Result:The contents of six heavy metals in Paridis Rhizoma met the ISO international standard of Heavy Metal Limit of Traditional Chinese Medicine-traditional Chinese Medicinal Materials. Under the limited value standard of Green Trade Standards of Importing Medicinal Plants and Preparations,the over-standard rate of heavy metal As was 15.4%,the excess rate of Cd was 5.1%,and the excess rate of Pb was 2.6%. The contents of Cu and Hg conformed to relevant requirements. Cluster analysis,statistical analysis and principal component analysis showed that for the same variety,differences in producing places had significant effects on heavy metal content,while differences in species had little effects. Conclusion:The results of this study indicated that the heavy metal content of Paris planted in and around Dali basically conformed to relevant standards. The differences of heavy metal content in Paris were mainly regional differences,which provided a theoretical basis for standardizing the cultivation of medicinal materials and formulating the limit standards of heavy metals for Paridis Rhizoma.
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OBJECTIVE: To explore the interference correction reduction method for the determination of cadmium(Cd), chromium(Cr), manganese(Mn), nickel(Ni) and lead(Pb) concentration in workplace air by inductively coupled plasma-atomic emission spectrometry(ICP-AES). METHODS: The interference sources in the determination of metals in workplace air with ICP-AES was analyzed. The results before and after the background correction or the internal standard calibration were compared. Linear regression is performed on the interference element mass concentration by interference error to obtain a table of interference factors. The measurement results of actual samples were corrected using background subtraction, internal standard correction, and interference factor method. RESULTS: The relative deviation of results and theoretical values without background subtraction were 219.5% and 131.5% for Cd and Pb, respectively. The relative deviation between the measured values and theoretical values was less than 10.0% after background subtraction. When the total metal ion concentration was >800.00 mg/L, the relative deviation between measured result and the theoretical values was-21.0%--11.0% without internal standard correction, and the absolute value of them were less than 10.0% after internal standard correction. The interference correction method was used to correct the concentration of Cd, Cr, Mn, Ni, Pb in welding smoke. The mass concentrations of Cd before and after interference correction were 3.90-32.50 and 1.20-7.10 μg/L, respectively. The mass concentrations of nickel before and after interference correction were 111.00-1 220.00 and 99.00-1 120.00 μg/L, respectively. The mass concentration of Cr,Mn and Pb remained unchanged before and after the interference correction. CONCLUSION: The background correction, internal standard correction and interference factor table can eliminate the interference for determination of metals in workplace air by ICP-AES and ensure the accuracy of results.
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A method for the determination of Fe, Co, Mn and Ni in synthetic diamonds by inductively coupled plasma atomic emission spectrometry ( ICP-AES) was proposed. The synthetic diamond sample was decomposed completely, while the sample was burned in air at 1000 ℃ for 10 h, and then a mixed acid of H2 SO4 , aqua regia and HClO4 was used for the dissolving the residue of the sample. In this method, the limits of detection of Fe, Co, Mn and Ni were 0. 0147, 0. 0018, 0. 0006 and 0. 0027 mg/L, respectively. Under the optimum condition, Fe, Co, Mn and Ni in synthetic diamond sample were determined. The values of RSDs (n=7) were less than 0. 5%. The recoveries of added standard were 94. 0%-105. 0%.
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A bismuth-antimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in copper-nickel sulfide ores was developed. 40. 0 g bismuth trioxide, 25. 0 g boric acid, 10. 0 g sodium carbonate and 1. 00 g starch were mixed with 10. 0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A two-step cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwave-digested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasma-atomic emission spectrometry ( ICP-AES), while 99 Ru, 103 Rh, 191 Ir were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), with 115 In, 185 Re as internal standard. RSD (n = 12) of the analysis results of five platinum group elements ( PGEs) in standard reference material GBW07196 ranged from 7. 04% to 9. 48% . Under the condition of 10 g sample, the detection limits (ng / g) for PGEs are 0. 027 for Ru, 0. 016 for Rh, 0. 11 for Pd, 0. 10 for Ir and 0. 11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
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An inductively coupled plasma mass spectrometry （ICP-MS） or inductively coupled plasma atomic emission spectrometry （ICP-AES） was developed to determine 19 elements in safflower, a traditional Chinese medicinal herb from Xinjiang Autonomous Region and Henan Province of China. Totally 19 elements in safflower included heavy metals, i.e. As, Cd, Cu, Hg and Pb, and wholesome elements, i.e. Al, Ca, Co, Cr, Fe, Mg, Mn, Mo, Ni, P, Se, Sr, V and Zn. The results showed that the concentrations of heavy metals in safflower samples were both low, all of which met the national hygiene standards except for Pb in Xinjiang sample. Meanwhile, the distribution tendency of elements in the two samples was similar, which indicated that the plant might absorb given elements in a proportional way. The method can be used for the quality control of elements in safflower, and it provides a way for the determination of the contents of safflower from Xinjiang and Henan.
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An inductively coupled plasma mass spectrometry (ICP-MS) or inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed to determine 19 elements in safflower,a traditional Chinese medicinal herb from Xinjiang Autonomous Region and Henan Province of China.Totally 19 elements in safflower included heavy metals,i.e.As,Cd,Cu,Hg and Pb,and wholesome elements,i.e.AI,Ca,Co,Cr,Fe,Mg,Mn,Mo,Ni,P,Se,Sr,V and Zn.The results showed that the concentrations of heavy metals in safflower samples were both low,all of which met the national hygiene standards except for Pb in Xinjiang sample.Meanwhile,the distribution tendency of elements in the two samples was similar,which indicated that the plant might absorb given elements in a proportional way.The method can be used for the quality control of elements in safflower,and it provides a way for the determination of the contents of safflower from Xinjiang and Henan.
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An inductively coupled plasma atomic emission spectrometry(ICP-AES) combined with a boron hydride vapour generation device was used for the determination of rhodium in waste catalyst. When the flow rate of sample and sodium borohydride solution was 2 mL/min, waste rate was 6 mL/min, the optimum conditions were as follows: 0.4 L/min of carrier rate, 1.0 mol/L of acidity of nitric acid for vapor generation and concentration of sodium borohydride 1.2(m/V). The study showed that a two-fold increase in the efficiency of rhodium was achieved as compared to nebulization. The detection limit was 6.9 μg/L, which is slight better than that of with nebulization. The linear range for rhodium was 20-1500 μg/L with a correlation coefficient of 0.9986. The mean recovery of sample analysis was 95.5%. Excellent agreement was found between the present method and FAAS.
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The pentavalent antimonies, mainly the meglumine antimoniate, are recommends as first-choice medicines for leishmaniasis therapy. In this work we described the development of formulations of meglumine antimoniate injectable medication, as well as the analytical methodology used in the selective determination of Sb(III) and Sb(Total) by hydride generation - inductively coupled plasma atomic emission spectrometry (HG-ICP-AES) and ICP-AES, respectively. On that purpose the analytical methodology was developed focusing on the HG-ICP-AES technique. The formulations using propylene glycol/water as vehicles in a 20:80 proportion were more appropriate for subsequent use in industrial scale. These formulations also showed a lower variation on Sb(III) percentage, no need of buffer solution to stabilize the formulation and no influence of the autoclaving in the quality of the product. The results of the development of the analytical methodology point out the proposed method as an efficient alternative for the determination of Sb(III) in the presence of large quantities of Sb(V) in injectable solutions of meglumine antimoniate, in a selective, linear, accurate and precise manner. In addition, the method showed a low limit of quantification, less interference of the matrix, and more resilience than batch techniques proposed in the Brazilian Pharmacopeia.
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Antimony/analysis , Antiprotozoal Agents/chemistry , Flow Injection Analysis/methods , Meglumine/chemistry , Organometallic Compounds/chemistry , Spectrophotometry, Atomic/methods , Antiprotozoal Agents/standards , Chemistry, Pharmaceutical/standards , Meglumine/standards , Organometallic Compounds/standards , Quality ControlABSTRACT
The aim of this study was to compare the compositions and cytotoxicity of white ProRoot MTA (white mineral trioxide aggregate) and 3 kinds of Portland cements. The elements, simple oxides and phase compositions of white MTA (WMTA), gray Portland cement (GPC), white Portland cement (WPC) and fast setting cement (FSC) were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES), X-ray fluorescence spectrometry (XRF) and X-ray diffractometry (XRD). Agar diffusion test was carried out to evaluate the cytotoxicity of WMTA and 3 kinds of Portland cements. The results showed that WMTA and WPC contained far less magnesium (Mg), iron (Fe), manganese (Mn), and zinc (Zn) than GPC and FSC. FSC contained far more aluminum oxide (Al2O3) than WMTA, GPC, and WPC. WMTA, GPC, WPC and FSC were composed of main phases, such as tricalcicium silicate (3CaO.SiO2), dicalcium silicate (2CaO.SiO2), tricalcium aluminate (3CaO.Al2O3), and tetracalcium aluminoferrite (4CaO.Al2O3.Fe2O3). The significance of the differences in cellular response between WMTA, GPC, WPC and FSC was statistically analyzed by Kruskal-Wallis Exact test with Bonferroni's correction. The result showed no statistically significant difference (p > 0.05). WMTA, GPC, WPC and FSC showed similar compositions. However there were notable differences in the content of minor elements, such as aluminum (Al), magnesium, iron, manganese, and zinc. These differences might influence the physical properties of cements.
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Humans , Agar , Aluminum , Aluminum Oxide , Calcium Compounds , Diffusion , Glutamates , Guanine , Iron , Magnesium , Manganese , Oxides , Plasma , Silicates , Spectrometry, X-Ray Emission , Spectrum Analysis , Zinc , PemetrexedABSTRACT
Objective To establish a new method for the determination of chromium (Ⅵ) in printing and dyeing wastewater. Methods A combined technique was employed for the determination of chromium (Ⅵ) by flow injection on-line separation and preconcentration on a micro column packed with alumina(acidic form) and inductively coupled plasma-atomic emission spectrometry (ICP-AES).The effect of acidity,concentration of eluent and coexistence ion on separation and enrichment was detected.Results The detection limit was 0.72 ?g/L.The LOQ was 2.38 ?g/L.RSDs were 1.45%～2.12%.The recovery rates were 96.0%-104.0%.The concentration enhancement of chromium (Ⅵ) was 10 times for 45 s sample loading.Analytic frequency was 33 samples one hour. Conclusion This method is sensitive,rapid and applicable to the determination of chromium (Ⅵ) in dyeing wastewater.
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Objective To study inductively coupled plasma atomic emission spectrometry(ICP-AES) used to determine blood boron(B),and to investigate the level of B in blood of children in Nanjing.Methods ICP-AES was applied to determine the level of B in the blood of 1032 healthy children and 1364 children patients after using 1mol/L HNO_(3) to treat whole blood.Results Precision of this method was 1.60%-4.31%,and recovery ratio was 93.3%-98.9%.The level of B in blood of the 1032 healthy children was(41.8?16.7)?g/L and that in blood of the 1464 patients was(25.1-58.5)?g/L(77%).Conclusion Precision and recovery ratio determined by the method are high,so it can be used as a reference method to detect the level of B in blood.And it preliminarily determines the reference levels of blood B of children in Nanjing as ranging from 25.1-58.5?g/L(except children below 1 year old).
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ve To study the new method for determination of chromium (Ⅵ) in waste water. Methods The chromium (Ⅵ) from waste water samples was seperated by ion-exchange method and concentrated, then was analyzed by inductively coupled plasma-atomic emission spectrometry. Results The precision, average recovery rate and detection limit were 2.05%, 99.7% and 0.018?g/ml respectively. Conclusion This method was easy and rapid to operate, and revealed less interference in determination of chromium (Ⅵ) in industrial waste water.
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0.999 5), RSD were no more than 3.0%. The recovery rates were 98.0%-102.0%. There was no significant difference between the results of this method and EDTA-Na2 titration. Conclusion The method is rapid, accurate, simple, little disturbance and is acceptable in determination of total hardness in drinking water.
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Seventeen trace elements, including twelve essential trace element, and three normal elements in serum of 417 healthy students aged 7 to 20 in Shanghai were analysed. Except Se which was determined by catalytic pulse polarography, Zn, Cu, Fe, Mn, Cr, Mo, Si, Sn, Ni, V, Co, Cd, Pb, Al, Ti, Sr, Ca, Mg and P in serum were measured by ICP-AES. The result showed that the distribution curve of normal elements and Zn, Cu in serum was more concentrated than the other trace elements. There were significant positive correlation between serum Zn, Fe, Mn, Sr and age, and negative correlation between Cu, Cr, Se, Pb and age, respectively. The elements of males were the same as that of females in total population, but the majority of the elements in serum had sex difference in different age-groups. The serum Cr, Si, Pb contents were higher, and Cu, Fe, Mn, Sr were lower in the urban than in the rural adolescents.