Determination of six heavy metals in peanuts using microwave-assisted digestion-inductively coupled plasma mass spectrometry with an octopole reaction system / 预防医学

Objective @#To establish a microwave-assisted digestion-inductively coupled plasma mass spectrometry (ICP-MS) with an octopole reaction system for simultaneous determination of six heavy metals in peanuts, including Cr, Ni, As, Cd, Pb, Hg. @*Methods @#Peanut samples were shelled and crushed evenly, and 0.350 0 g was accurately weighed and digested with 5 mL nitric acid and 1 mL hydrogen peroxide in a digestion tank. Following microwave-assisted digestion, pure water was used to quantify the samples, and internal standards and an octopole reaction system were used to remove the interference. Then, the contents of six heavy metals were determined in peanuts by ICP-MS. The accuracy and precision of ICP-MS were evaluated using national criteria ( GBW 10013 and GBW 10044 ) and spike-and-recovery testing. @*Results @#The six heavy metals showed good linearity at the selected linear range ( r≥0.999 8 ). The detection limits of ICP-MS ranged from 0.001 4 to 0.023 8 ng/mL, and the spike-and-recovery rates ranged from 94.7% to 98.8%, with the relative standard deviations ranging from 0.7% to 3.6%. In addition, the determination results of the standard reference materials were all within the normal reference range. The detection of six heavy metals was 100.0% in 60 peanut samples, and the contents of six heavy metals were all low.@*Conclusion @#The established ICP-MS assay is feasible for simultaneous determination of multiple heavy metals in peanuts.

Establishment and optimization of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of aluminum residues / 中国输血杂志

【Objective】 To establish and optimize a method for the determination of aluminum (Al) residue by inductively coupled plasma mass spectrometry (ICP-MS). 【Methods】 Nitric acid solution was used to treat samples and standards. The concentration of nitric acid solution and equipment parameters were optimized, and the specificity, linearity, repeatability, accuracy, detection limit, quantitative limit and intermediate precision of the optimized detection method were investigated to confirm whether it was suitable for the determination of Al residue in human serum albumin. 【Results】 The concentration of nitric acid was 5%, and digest time was 4 h. The equipment condition of ICP-MS was as follows: RF power: 1600 W, sampling depth: 10 mm, atomizer / carrier gas flow rate: 1.0 L/ min, compensation flow rate: 0.5 L/ min, experimental mode: standard mode, integration time: 0.2 s, data acquisition: 3 times. Specificity: The recoveries of Al: 92% (high concentration, RSD=3.5%), 98% (low concentration, RSD=4.9%). Linearity: In the range of (0~40) μg/L, the correlation coefficient between concentration and optical energy signal (CPS) of standard / sample were higher than 0.999 0. Accuracy/ Repeatability: The recoveries of sample (3 concentration): 108% (RSD=4.7%), 110% (RSD=4.9%) and 110% (RSD=2.8%). The detection limit was 0.006 μg/L, and the quantitation limit was 0.019 μg/L. Intermediate precision: personnel factor and date factor, P>0.05, RSD (12 times)=2%. Comparison between ICP-MS and atomic absorption spectrometry (AAS): the deviation between ICP-MS and AAS was 8%, and that of samples was 3%, with no significant difference noticed between the two methods. 【Conclusion】 After optimization, ICP-MS method has shown good performance in terms of specificity, linearity, repeatability, accuracy, detection limit, quantitative limit and intermediate precision, and is suitable for the determination of Al residue in human albumin products of our company.

Detecting 12 elements in human biological samples by ICP-MS method / 中国职业医学

OBJECTIVE: To establish a method for detecting the contents of 12 toxic elements such as beryllium,vanadium and thallium in human whole blood,urine and hair by inductively coupled plasma-mass spectrometry( ICP-MS).METHODS: Whole blood( 0.25 mL) and urine( 10.00 mL) were diluted 20 times into suspension by 0.1% TritonX-100 + 0.5% nitric acid,and analyzed by ICP-MS.The hair( 0.20 g) was mixed with nitric acid and digested by microwave,then made up to 10.00 mL with purified water.The analysis was performed by ICP-MS.RESULTS: The linear correlation coefficients of all the 12 elements,such as beryllium,vanadium,chromium,manganese,cobalt,nickel,arsenic,cadmium,tin,antimony,tellurium and lead were≥0.999 5.The detection limit for whole blood and urine was 0.097-1.995 μg/L,and the detection limit for hair was 0.001-0.012 μg/g.The recovery rates for whole blood,urine and hair were 92.3%-105.0%,93.7%-115.5% and 92.5%-111.0%,respectively.The within-run relative standard deviation( RSD) were 0.7%-5.8%,0.8%-4.6% and 2.2%-8.4%,respectively; the between-run RSD were 1.6%-7.1%,3.5%-7.5% and 2.8%-8.8%,respectively.CONCLUSION: This method has good accuracy,high sensitivity and good precision,which is suitable for rapid screening for various elements in human biological samples.

Laser Ablation-Inductively Coupled Plasma-Mass Spectrometer:A Quantification Strategy Based on Two Reference Materialsand Bulk Normalization as 100% (wt) / 分析化学

Quantitative calibration strategy as an essential issue in laser ablation ICP-MS plays an important role for the guarantee of analytical accuracy.In this study, uncertainties of reference values in current available glass certified reference materials (NIST, MPI-DING and USGS) as well as the matrix effect among them were systematically evaluated.The results illustrated that NIST610 was better than other reference materials from aspect of reference value uncertainty.The matrix effect among NIST, MPI-DING and USGS reference materials was insignificant under our experimental conditions.A quantification strategy based on two reference materials (NIST610 and StHs6/80-G) and normalization to 100% (w/w) was proposed to avoid the insufficiency of single reference material strategy, which suffered the very low content and large uncertainty for some elements.The comparision of ML3B-G results obtained from three quantification strategies (single reference material NIST610, single reference material StHs6/80-G and two refterence materials) illustrated that the proposed strategy improved the analytical accuracy.Three reference materials (BCR-2G, CGSG-2 and KL-2G) were quantified with the proposed strategy, and almost all data matched well with reference value, meanwhile the data reported here could supplement the reference value database.

Rapid Determination of Fifteen Elements in Ibuprofen Injection by ICP-MS / 中国药师

Objective:To develop a method for the rapid determination of 15 elements such as Al,Ca,Cr,Mg,Zn,K,B,Sr, Cd,Ba,Pb,As,Sb,Na and Li in ibuprofen injection by ICP-MS. Methods:After diluted by 2% nitric acid solution,the samples was determined directly by inductively coupled plasma mass spectrometry(ICP-MS)with the online internal standard to correct matrix interference and signal drifting. Results:The detection limits of the method were ranged from 0. 031 to 5. 1 μg·L-1 . The average recoveries were within the range of 82. 6% -107% and RSDs were all less than 5% . Conclusion:The method is rapid, accurate and highly sensitive,which can provide technical support for the quality control of ibuprofen injection.

The Analysis Methodology for Multiple Elements in Four Herbs ofSanjie Zhentong Capsules / 世界科学技术-中医药现代化

To develop a method for the determination of 18 elements such as Pb, Cu, As, Hg, Mn, Ni, & Tl in Panax notoginseng,Bulbus fritillariae thunbergii,Coix seed, Resina draconis, and to control the contents of heavy metal elements in Sanjie Zhentong Capsule, the samples were digested by microwaves and then analyzed by appropriate determination parameters through ICP-MS, with the internal standard method to improve the matrix effect and interference. The correlation coefficientR2≥ 0.999 2. The lowest limits of quantification were from 0.002 8 to 0.54 μg·L-1. The experiments had better repeatability, while the recovery values ranged from 73.01% to 109.13%. The method is simple, accurate and high sensitive, and it can be used for the determination of rapid monitoring the multi-elements inPanax notoginseng, Bulbus fritillariae thunbergii, Coix seed,and Resina draconis.

Investigation of relationship between schizophrenia and ten kinds of elements in serum / 中国生化药物杂志

Objective To study the relationship between the changes of ten elemental contents in serum and schizophrenia.Methods Calcium (Ca), magnesium (Mg), zinc (Zn), iron (Fe), aluminum (Al), arsenic (As), selenium (Se), copper (Cu), lead (Pb), manganese (Mn) in serum in the of schizophrenic patients and normal subjects are measured by inductively coupled plasma mass spectrometer and inductively coupled plasma emission spectrometer, compared the content of elements between the schizophrenia and normal.Results There were significant differences ( P<0.05) in other elements between two groups except lead.The contents of Ca,Fe,Mg,Zn,As,Se,Cu in the patients with schizophrenia were significantly lower than those in control, while Al, Mn were significantly higher than those in control.Most of elements in serum between case and control groups were correlated (P<0.05).Some of element ratios which have physiological significance were significant statistically (P<0.05), such as: Ca/Mg, Ca/Fe and so on.Conclusion These findings suggest that the patients with schizophrenia might have an abnormal elemental metabolism.Given the relationship among the elements, the element ratios are more valuable in reflecting the relationship between schizophrenia and elements.