Preliminary evaluation of a microwave-assisted metal-labeling strategy for quantification of peptides via RPLC–ICP-MS and the method of standard additions
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Identification and quantification of human fingernail calcium is demonstrated by laser-induced breakdown spectroscopy (LIBS) using the modified external standardization. Since cow’s horn and hoof have structures very similar to the fingernail, either of them is individually selected as the matrix of standard samples. In total, 12 standard samples for each matrix are prepared using CaCO3 as the standard substance. In order to achieve accurate calibration curves associated with the method of modified external standard, foremost, the calcium concentration of each of matrices (horn and hoof) is determined by the method of standard additions. The results indicate that there exist 4887 µg/g (ppm) and 4156 µg/g (ppm) of calcium in the pure horn and hoof matrices, respectively. Then, the external calibration curves related to the two matrices are plotted using the information of standard samples. Finally, by the use of signals obtained from LIBS experiment for three different fingernails and inserting their amounts into the calibration curves, the calcium concentration of the fingernails under test is measured to be 10,814 µg/g (ppm), 13,106 µg/g (ppm) and 14,974 µg/g (ppm). The difference of the calcium concentrations between three specimens, as will be discussed, may be due to different physical conditions of people who have donated their fingernails.
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The measurement uncertainty related to the analysis of eight trace elements (Pb, Zn, Cr, Mn, Cu, Cd, Hg and As) in drinking water using Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) was evaluated in detail.
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The quantitation of target analytes in complex matrices such as biological samples requires special calibration approaches to compensate for additional capacity or activity in the matrix samples. A conventional calibration curve, obtained with standard solutions, is one of the most important calibration procedures for quantitation of target analytes in such matrices. However, these technique require a great number of reagents and material, and consume a considerable amount of time throughout the analysis. In this work, a new calibration procedure to analyze urine samples is proposed for the first time in chromatography procedures. The proposed calibration, called the addition calibration technique, was used for the determination of acetaminophen and hydrochlorothiazide in urine samples. The results obtained for the proposed calibration mode were compared to those obtained using standard addition and standard calibration techniques. The proposed addition calibration was validated by statistical studies between results obtained by the addition technique and conventional techniques, using the ANOVA test and linear regression. The results demonstrated good agreement among them. The performance of the analytical method was evaluated. Relative standard deviation, limit of detection, and limit of quantification are respectively 0.5–0.6%, 0.169–0.75 µg/mL, and 0.565–2.5 µg/mL. Linear range falls within the range of 0.3 to 63.8 µg/mL for both compounds. Accuracy ranged between 94% and 101%.
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OBJECTIVE To establish a rapid and accurate method for instantaneous analysis of Pb,Cd,As in blood by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). METHODS The assay method was established according to comparative study of standard curve method and standard addition curve method (a method derived and developed from standard addition method). RESULTS Both methods showed good correlative coefficients of calibration curve,limits of detection and reproducibilities for all test elements. Standard curve method,indicated unsatisfactory spiked recovery between 92.00% and 135.0%,as well as unacceptable determined values of reference materials (GBW09139e and GBW09140e). Standard addition curve method indicated satisfactory spiked recovery range from 93.33% to 102.0% and coincident contents of reference materials. CONCLUSION Standard addition curve method,bearing better spiked recovery and precise than those of standard curve method,was a rapid and accurate method for simultaneous determination of harmful elements in blood by ICP-MS.
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A method of inductively coupled plasma mass spectrometry (ICP-MS) was established to determinate trace impurity elements in chitosan. After dissolving in 3% citric acid and low concentration of HCl, the elements including Be, B, Na, Mg, P, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Cd, Sn, Sb, Hg and Pb in chitosan were measured with ICP-MS directly. The addition of low concentration of HCl could effectively improve the stability of all elements, especially Hg and Sn. Dynamic reaction cell (DRC) was used to correct the interference of chlorine ion and other mass spectral interference. The matrix matching and the internal standard elements mixed solution (Sc, Y, In and Bi) had compensated the difference of sample transfer efficiency and evaporation rate of organic solvent. Under the optimum condition, the standard curve of each element exhibits linear correlation coefficient was not less than 0.999 7. The detection limit of the 20 elements was in the range of 0.6～19.0 ng·L-1 while the recovery of standard addition was 89.50%～109.00% with RSD 1.17%～4.05%. The practical sample analysis results showed that the content of impurities in food grade chitosan is very low. And the heavy metal content is extremely low and safe to eat. This method is very simple, sensitive and accurate for the determination of 20 impurity elements in the food grade chitosan.
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The standard solutions prepared by different methods to establish the amount of external standard calibration curve recovery compared to the preparation of acetone solvent matrix calibration curve standard solution of chlorpyrifos recovery is 92%to 99%.relative standard deviation(RSD)≤4.18%,chlorpyrifos in the 0.035～1.4 mg/L in the range a good linear relationship between the instrument detection limit of this method is 0.02 mg/L,the detection limit is 0.008 mg/kg.On the same sample by double flame photometric detector(FPD)detection, DB-1701+DG than the DB-1 column matrix effects a small column.Standard solution prepared by the solvent matrix to establish the amount of external standard calibration curve to eliminate matrix effects.
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The preparation of calibration curves using an aqueous standard solution was studied for the direct determination of trace levels of zinc in high-purity iron and steels by graphite furnace atomic absorption spectrometry (GF-AAS) using solid sampling technique. Certified reference materials of high-purity iron and steel samples were used to confirm the trueness of the proposed methods. The standard addition method for the solid sampling technique that we have proposed gave accurate analytical results. The calibration curve prepared by the standard addition method can be used as a kind of iron-matrix matching calibration curve, and it provides rapid and accurate determinations of zinc. The detection limit of zinc in iron and steel samples was 0.86 mg kg−1 when 15 mg of one sample was measured.
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Inductively coupled plasma mass spectrometry (ICP-MS) can be used to detect metal elements existing in samples. Because we are not capable of conducting ICP-MS on our own, we must seek help from our advisors. This protocol is a general description of our actions.
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