A comparative study of iodine content in serum, plasma and whole blood / 中华地方病学杂志

Objective:To evaluate the consistency of individual iodine nutrition levels by serum iodine, plasma iodine and whole blood iodine, and to provide reference for iodine-related epidemiological investigation.Methods:Healthy adults aged 18 - 59 years were recruited from the Research Center of Environment and Health in Water Source Area of South-to-North Water Diversion of Hubei University of Medicine. Whole blood sample was collected and serum and plasma were separated. The content of iodine in serum, plasma and whole blood was determined by inductively coupled plasma mass spectrometry (ICP-MS), and the linear relationship, precision and accuracy of the standard curve of the detection method were evaluated. The difference of three kinds of blood iodine levels was analyzed by variance analysis of compatibility group design, and Passing-Bablok regression and Bland-Altman plot were used to evaluate the consistency between serum iodine and plasma iodine.Results:The linear range of iodine in serum, plasma and whole blood was 0.0 - 25.0 μg/L, and the correlation coefficients ( R2) were all > 0.999. The relative standard deviation of 8 mixed blood samples ranged from 1.9% to 4.3% ( n = 6), and the determination results of blood iodine certified standard substances were all within the reference range. The recovery rate of the added standard ranged from 99% to 106%. The iodine levels in serum, plasma and whole blood of 50 volunteers were (57.31 ± 8.06), (57.49 ± 8.50) and (33.89 ± 5.40) μg/L, respectively, and there was no statistically significant difference between serum iodine and plasma iodine ( P = 0.904). The results of Passing-Bablok regression showed that there was no statistically significant difference in bias between serum iodine and plasma iodine ( P = 0.538). The Bland-Altman plot indicated that the difference between serum iodine and plasma iodine was within the consistency limit. Conclusion:The results of plasma iodine and serum iodine are in good agreement, and plasma iodine can be used as an evaluation index of individual iodine nutrition level. But there is no consistency between whole blood iodine and serum iodine.

Determination of iodine in workplace air by inductively coupled plasma mass spectrometry / 中国职业医学

Objective To establish a solvent desorption inductively coupled plasma-mass spectrometry (ICP-MS) method for determination of iodine in workplace air. Methods Iodine in workplace air was collected with alkaline activated carbon tube and desorbed with 10.0 mL pure water or 20 mmol/L sodium bicarbonate solution. Rhenium-185 was used as an internal standard for quantification. The sample was determined in standard mode and kinetic energy discrimination collision (KED) mode by ICP-MS. Results In standard mode, iodine showed a good linear range in the concentration of 9.0 to 1 100.0 μg/L, with a correlation coefficient of 0.999 3 and a detection limit of 2.7 μg/L. In KED mode, iodine showed a good linear range in the concentration of 24.3 to 800.0 μg/L, with a correlation coefficient of 0.999 1 and a detection limit of 7.3 μg/L. The average desorption efficiency using pure water ranged from 99.1% to 106.7%, with within-run relative standard deviation (RSD) of 3.1% to 8.0% and between-run RSD of 4.9% to 9.3%. The average desorption efficiency using sodium bicarbonate solution ranged from 96.5% to 105.3%, with within-run RSD of 4.9% to 8.6% and between-run RSD of 2.5% to 9.9%. There were no statistical significant differences in the main effects of desorption solution, ICP-MS detection mode, their interaction on average desorption efficiency and within-run RSD (all P>0.05). Samples could be stored at room temperature for at least 7 days. Conclusion This method is highly sensitive, accurate, and suitable for the determination of iodine in workplace air. The sample pretreatment is simple and rapid.

Determination of thallium and its soluble compounds in workplace air by inductively coupled plasma mass spectrometry / 中国职业医学

Objective To establish a method for the determination of thallium and its soluble compounds in workplace air using microporous filter membrane sampling and inductively coupled plasma mass spectrometry (ICP-MS). Methods Thallium and its soluble compounds in workplace air were collected using microporous filter membranes, digested with nitric acid, quantified using lutetium internal standard method, and detected by ICP-MS. Results The linear range of thallium was 0.00 to 600.00 μg/L, with the correlation coefficient of 1.000. The detection limit was 0.08 μg/L, and the lower limit of quantification was 0.26 μg/L. The minimum detection concentration and minimum quantitation concentration of thallium of 75.00 L workplace air were 1.0×10-5 and 3.0×10-5 mg/m3, respectively. The minimum detection concentration and minimum quantitation concentration of thallium of 480.00 L workplace air was 2.0×10-6 and 5.0×10-6 mg/m3, respectively. The recovery rate of spiking was 100.82%-103.44%, and the relative standard deviation within- and between-batches was 1.50%-3.32% and 1.32%-3.11%, respectively. The sample could be stored at room temperature for at least 14 days. Conclusion This method can be used for the detection of thallium and its soluble compounds in workplace air.

ICP-MS establishes blood lead reference method expected to improve detection accuracy / 中华检验医学杂志

Lead poisoning severely threatens human health with its cumulation and durability in the body. The analysis of lead in blood is vital for screening, diagnosis, treatment, and prognostication of lead poisoning and for indirectly monitoring the level of lead in the environment. Although the detection programs are available throughout our country, the accuracy and comparability of the results cannot meet the expectation. A variety of factors can affect the accuracy of blood lead testing. To promote the application of blood lead analysis in clinical trials and reduce the bias of results, a better reference system for blood lead analysis should be established to evaluate the accuracy of traditional methods, promote the standardization of blood lead analysis and achieve accurate blood lead testing.

Determination of lead isotope ratios by inductively coupled plasma mass spectrometry and comparison of lead isotope ratios among different samples / 环境与职业医学

background The lead isotope ratios (LIR) differ among different sourced samples. Previous domestic and oversea studies on source tracing by LIR in human blood or urine mainly focused on the comparison of blood or urine samples from the same or different individuals, while few comparisons between biological and environmental samples, and the reported relative standard deviations (RSDs) of the main LIR (207/206Pb and 208/206Pb) fluctuate widely from 0.3% to 1%. Objective To optimize inductively coupled plasma mass spectrometry (ICP-MS), obtain a better RSD, and determine LIRs of human blood, urine, and related environmental samples. Methods The ICP-MS was optimized for operating conditions and parameters according to the sensitivity and RSD of LIR. The study subjects were 40 lead-exposed workers in a lead-acid battery factory and 2 lead poisoned children in a hospital. The samples included 40 blood and 40 urine samples from the workers before shift, 4 dust samples and 2 water samples in the workplace on the same day before shift, 2 blood and 3 urine samples from the children before hospital admission due to lead-poisoning, and 4 urine samples after medical treatment. After heating and acid digestion, the LIR (207/206Pb and 208/206Pb) of biological and environmental samples were determined by the optimized ICP-MS method. t-test and two-dimensional traceability graphics were adopted to analyze the detection results. Results The calibrated RSDs of the LIR (207/206Pb and 208/206Pb) of lead isotope standard solution were 0.11% and 0.08% respectively, and the NIST-SRM-981 actual values were 0.91531±0.00097 and 2.1670±0.0017, respectively. When the total concentration of lead was greater than 5 μg·L−1, the RSD of each isotope ratio was stable gradually; when the total concentration of lead was between 10-80 μg·L−1, the RSD was below 0.20%. There were statistically significant differences in the blood and urine LIR (207/206Pb and 208/206Pb) of the lead-exposed workers (t=5.831, P<0.001; t=21.021, P<0.001), the LIR (207/206Pb and 208/206Pb) between workplace dust samples and workers’ urine samples (t=−6.879, P=0.038; t=12.521, P<0.001), and the 208/206Pb between workplace dust samples and workers’ blood samples (t=−10.46, P<0.001), except the 207/206Pb between workplace dust samples and workers’ blood samples (t=−0.12, P=0.912). In the patients afflicted with lead poisoning, the projection points of LIR of blood and urine samples from the same individual were not at the same level in the two-dimensional model, nor was the LIR of urine samples before and after medical treatment of the same individual. Conclusion The optimized ICP-MS can control the RSD of main LIR (207/206Pb and 208/206Pb) below 0.20%. There are differences in the LIR distributions of different samples.

Identification of Growth Years of Scutellariae Radix By Characteristic Spectrum of Inorganic Elements Combined with Chemometrics / 中国实验方剂学杂志

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.

Analysis of heavy metal pollution in Lonicerae Japonicae Flos and its health risk assessment / 中国中药杂志

In this study, the content of five heavy metals(Pb, Cd, As, Hg, and Cu) in 59 batches of Lonicerae Japonicae Flos(LJF) medicinal materials and pieces were determined by inductively coupled plasma mass spectrometry(ICP-MS). The health risk assessment was processed using the maximum estimated daily intake(EDI), target hazard quotients(THQ), and carcinogenic risks(CR) assessment models. With reference to the limit standard for heavy metal content in LJF specified in 2020 edition of Chinese Pharmacopoeia, five batches produced in Hebei were found to contain excessive Pb, and the remaining 54 batches met the specifications, with the unqualified rate of 8.47%. Comparative analysis of heavy metal content in LJF samples from three different producing areas, namely Shandong, Henan, and Hebei showed that the levels of Pb, As, and Hg in LJF from Hebei were significantly higher than those from Henan and Shandong. The samples produced in Shandong contained the highest content of Cd. The samples from Hebei contained the highest content of Cu while those from Shandong had the lowest content of Cu. As demonstrated by health risk assessment based on the EDI, THQ and CR models, these 59 batches of LJF samples did not cause significant health hazards for the exposed population, and there was no potential non-carcinogenic or carcinogenic risk. In conclusion, a few of LJF samples contained excessive heavy metals, so some measures, including controlling production environment, cultivating management mode, and optimizing processing methods, should be taken for ensuring the medication safety of LJF.

Determination of 17 elements in placenta by microwave digestion-inductively coupled plasma mass spectrometry / 预防医学

Objective@#To establish a microwave digestion-inductively coupled plasma mass spectrometry assay for simultaneous determination of multiple elements in placenta.@*Methods@#Fresh placental tissues were dried at 60 ℃ for 15 h and ground into power. Then, 0.3 g homogenized samples were digested in a microwave digestion system. The interference from mass spectrometry was removed using the kinetic energy discrimination model in the inductively coupled plasma mass spectrometry, and the baseline interference was removed by online internal standards. The contents of 17 elements were determined in placental specimens using the established microwave digestion -inductively coupled plasma mass spectrometry assay, including V, Ni, Co, Fe, Cr, Cu, Zn, Mn, As, Sn, Sb, Ba, Se, Cd, Pb, Hg and Tl.@*Results@#Good linearity was shown for V, Ni, Co, Cr, As, Se, Cd, Pb and Tl at 1 to 50 µg/L, Fe at 100 to 5 000 µg/L, Zn, Cu, Mn and Ba at 10 to 500 µg/L, Sn and Sb at 0.1 to 5 µg/L, and Hg at 0.2 to 2 µg/L, with all correlation coefficients of 0.999 8 and higher. The detection limits of these 17 elements ranged from 0.5 to 100 μg/kg, with relative standard deviations of 2.1% to 6.5%, and recovery rates of 83.3% to 110.0%. The determination results of 17 elements were all within the normal reference range defined in the certified reference materials of chicken (GBW10018). @*Conclusions@#The microwave digestion-inductively coupled plasma mass spectrometry established based on optimized pretreatments and mass spectrometry detection conditions, is feasible for simultaneous determination of multiple elements in placenta.

In vivo and in vitro inductively coupled plasma mass spectrometry quantification of minerals and heavy metals in Qishiwei Zhenzhu pill and their effect on intestinal flora / 中国药理学与毒理学杂志

OBJECTIVE Cerebral ischemia or ischemic stroke is due to insufficient blood supply to the brain, which causes hypoxia or ischemia in some areas. This work aimed to quantify the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro, analyze its effect on the types and abundance of intestinal flora, and study its mechanism on inflammation and apoptosis pathways as a treatment for cerebral ischemia. METHODS Microwave digestion and induc?tively coupled plasma mass spectrometry (ICP-MS) were used to determine the minerals and heavy metals in 10 batches of Qishiwei Zhenzhu pill in vitro. With the use of the middle cerebral artery obstruction (MCAO) model, ICP-MS was applied to determine the content of minerals and heavy metals in hepatic portal vein blood, abdominal aortic blood, brain, liver, kidney, hair, urine and feces at different time periods. On this model, the ileum, cecum, and colon tissues were tested for intestinal pathology, and 16S rRNA was used for sequencing. Species taxonomy, α diversity, and spe?cies microbial composition and structure analysis were also performed. Polymerase chain reaction and Western blotting were employed to determine the mRNA and protein expression of p38 MAPK, caspase-3, IL-1β and TNF-α in the isch?emic brain tissues of rats. RESULTS The average content of heavy metals in the 10 batches of Qishiwei Zhenzhu pill samples is in the descending order Hg>Cu>Pb. Significant differences in the metal elements are found among Qishiwei Zhenzhu pill from different manufacturers but not among the different batches of the same manufacturer. An extremely low content of heavy metals are absorbed into the blood or accumulated in the brain, liver, kidney, and other tissues. Stool is the main excretion route of minerals and heavy metals from Qishiwei Zhenzhu pill. This medicine helps repair the intestinal mucosa in MCAO rats. At the phylum level, it can regulate the abundance of Firmicutes and Proteobacteria in the intestinal flora of rats with cerebral ischemia. At the genus level, it can adjust the abundance of Escherichia Shigella. At the species level, it can adjust the abundance of Lactobacillus yoelii and Lactobacillus reuteri. Cluster classification results show that Qishiwei Zhenzhu pill can improve the intestinal flora of rats with cerebral ischemia, reduce the mRNA and protein expression of caspase-3 and IL-1βin rat brain tissues, and have a tendency to decrease the mRNA expres?sion of p38 MAPK and TNF-α. CONCLUSION Quantifying the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro will help improve their quality standards. Minerals and heavy metals are mainly excreted in feces, accumu?late in extremely low levels in various tissues, and do not damage the intestinal mucosa. The effective material basis of Qishiwei Zhenzhu pill in treating cerebral ischemia may be related to their Li, Cr, and Cd elements. These pills can improve the environment of intestinal flora, and their mechanism of treatment for cerebral ischemia may be related to the down-regulation of IL-1βinflammatory factor and inhibition of cell apoptosis.

Heavy Metal Analysis and Evaluation of Geotechnical Plant System of Dendrobii Officinalis Caulis in Typical Karst Area / 中国实验方剂学杂志

Objective:To systematically evaluate the safety of heavy metals in Dendrobii Officinalis Caulis and its rhizosphere soil and bedrock in epiphytic culture imitated wild rock fissure. The distribution characteristics of heavy metals in carbonate-black limestone-Dendrobii Officinalis Caulis system in the study area were analyzed. Method:Samples of biennial Dendrobii Officinalis Caulis， black calcareous soil and carbonate rocks were collected from fracture-epiphytic culture in karst area of Guizhou province. The contents of Cu， Pb， As， Cd in Dendrobii Officinalis Caulis， and Cu， Pb， As， Cd， Cr in soil and bedrock were determined by inductively coupled plasma-mass spectrometry （ICP-MS）. The detection conditions were as follows：plasma power of 1 550 W， feedback power of 2 W， sampling depth of 9 mm， atomization chamber temperature at 2 ℃， analysis mode of full quantitative， and double charge of <1.5%. Hg content in Dendrobii Officinalis Caulis was determined by atomic fluorescence spectrometry， and Hg content in soil and bedrock was determined by mercury analyzer. SPSS 26.0 software was used to analyze the test data. Result:The contents of Cu， Pb， As， Cd and Hg in Dendrobii Officinalis Caulis were all within the safety threshold. The contents of Pb， As， Cd， Hg and Cr in black calcareous soil were higher than the corresponding background values of Chinese soil （<italic>P</italic><0.05， <italic>P</italic><0.01）， Cd in black calcareous soil was slightly polluted， while Cr， Cu， As， Pb and Hg were clean. The contents of Cu， As， Pb， Cd， Hg and Cr in carbonate rocks were significantly lower than those in black calcareous soil （<italic>P</italic><0.01）. The order of heavy metals in black calcareous soil affected by parent rock was Hg>Cd>Cu>As>Cr>Pb. The bioconcentration factor （BCF） of heavy metals in Dendrobii Officinalis Caulis was in the order of Cu>Cd>Pb=Hg>As， but the BCFs of these five heavy metals were all low （all <10%）. The contents of Cu， Pb， Cd and Hg in Dendrobii Officinalis Caulis increased slightly with the increase of heavy metal content in the rhizosphere soil， while the content of As decreased with the increase of As content in the rhizosphere soil. In addition to Cu content in Dendrobii Officinalis Caulis， the migration characteristics of Pb， As， Cd and Hg in the system of carbonate-black limestone-Dendrobii Officinalis Caulis showed consistency. Conclusion:The distribution characteristics of heavy metals in geotechnical plant system in the study area show obvious inheritance. The characteristics of high content， low activity and low pollution risk of heavy metals in black limestone soil and low BCF are the main factors affecting the safety threshold of five heavy metals in Dendrobii Officinalis Caulis.

Determination of lithium and its compounds in workplace air by inductively coupled plasma-mass spectrometry / 中国职业医学

OBJECTIVE: To evaluate the suitability of two pretreatment methods, the nitric acid digestion method and the elution method, and two measurement modes of inductively coupled plasma-mass spectrometry(ICP-MS), the No gas mode and the helium collision(He) mode, for the determination of lithium and its compounds in the workplace air. METHODS: We collected lithium and its compounds in the air of the workplace using the microporous filter membrane, and two pretreatment methods, the nitric acid digestion and elution methods were used for processing, and measured with the No gas mode and the He mode of ICP-MS. RESULTS: The good linearity range of lithium concentration in No gas mode and He mode of ICP-MS method was 0.00-500.00 μg/L, and the correlation coefficient was 0.999. The detection limit and the lower limit of quantification of lithium were 0.04 and 0.13 μg/L respectively in the No gas mode. In He gas mode: they were 0.12 and 0.39 μg/L respectively. Using the nitric acid digestion method for pre-treatment, the recovery rate of lithium addition was 96.9%-104.9%; the within-run and the between-run relative standard deviations were 3.3%-5.0% and 2.9%-5.3% respectively. Using the elution method for pre-treatment, the recovery rate of lithium addition was 97.6%-102.1%; the within-run and the between-run relative standard deviation were 3.3%-4.6% and 3.4%-4.8%, respectively. The sample could be stored at room temperature for at least 14 days. CONCLUSION: The ICP-MS method can be used as a new technology for detecting lithium and its compounds in the air of workplace. It is recommended that the elution method and the No gas mode be the first choice when measuring lithium and its compounds.

Detecting 41 mineral elements in human whole blood by inductively coupled plasma-mass spectrometry / 中国职业医学

OBJECTIVE: To establish a method for detecting 41 mineral elements such as beryllium, magnesium and calcium in whole blood by inductively coupled plasma-mass spectrometry(ICP-MS). METHODS: After the whole blood samples were diluted 1∶20 in a mixed solution containing 0.10% Triton X-100 and 0.50% nitric acid, 41 mineral elements in whole blood samples such as beryllium, magnesium and calcium were determined by the ICP-MS, using scandium, rhodium and iridium as the internal standard elements. RESULTS: The linear correlation coefficient was >0.999 0 in these 41 elements such as beryllium, magnesium and calcium in the whole blood. The detection limit was 0.006-247.000 μg/L, the quantification lower limit was 0.020-822.000 μg/L. The recovery rate of standard addition was 84.00%-109.40%. The within-run and between-run relative standard deviation were 0.66%-7.34% and 0.56%-8.22%, respectively. The samples could be stored at-20 ℃ for at least 14 days. CONCLUSION: This method is simple, rapid and sensitive, with good precision and reliable results. It can be used for detecting multiple mineral elements in whole blood of normal and occupational population.

Uncertainty evaluation of total arsenic in pork by inductively coupled plasma mass spectrometry / 上海预防医学

Objective To make uncertainty evaluation of total arsenic in pork by using the national food safety standard "GB 5009.11-2014 determination of total arsenic and inorganic arsenic in food", and discuss the influence of each uncertainty component on the determination results so as to improve the accuracy of the experimental results. Methods The uncertainty sources that affected the measurement results in the measurement process, including repeatability measurement, sample weighing, sample dilution, standard concentration, standard curve and so on were evaluated.The uncertainty introduced by the repeatability measurement was evaluated by class A, the uncertainty caused by other factors was evaluated by class B, and the phase was calculated according to each component.The synthetic standard uncertainty and the relative expanded uncertainty were discussed, and so were the influence of the uncertainty components on the measurement results. Results According to the contribution of uncertainty from large to small was the sample standard concentration, standard curve, repeatability determination, sample weighing and sample dilution.The calculated relative composite standard uncertainty was 0.0405, and the relative expanded uncertainty was 0.081 (k=2). Conclusion The experimental results show that the concentration of standard substance has a great influence on the measurement process, so it is necessary to standardize the dilution process and simplify the dilution procedure to improve the accuracy of measurement results.

Simultaneous Determination of 14 Elements in Deproteinized Calf Blood Extractives Injection by ICP-MS / 中国药房

OBJECTIVE： To establish a method for the content determination of 14 elements in Deproteinized calf blood extractives injection. METHODS： Inductively coupled plasma-mass spectrometry （ICP-MS） was adopted. The radiofrequency power was 1 350 W； flow rate of carrier gas （argon） and collision gas （helium） was 1.1 L/min and 4.5 L/min respectively； integration time was 1.5 s； plasma gas flow rate was 18 L/min； depth of sampling was 65 mm； speed of sampling peristaltic pump was 24.0 r/min； data sampling mode was peak-jump acquisition mode； data collection was repeated for 3 times. RESULTS： The linear ranges of Cd， Pb， As， Co， V， Ni， Tl， Ag， Mo， Cu， Cr， Ba and Al were 0.05-50 μg/L （r＝0.999 7）， 0.05-50 μg/L （r＝0.999 7）， 0.05-50 μg/L （r＝0.999 8）、0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 8）， 0.05-50 μg/L （r＝0.999 6）， 0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 8）， 0.05-50 μg/L （r＝0.999 6）， 0.05-50 μg/L （r＝0.999 6）， 0.05-50 μg/L （r＝0.999 7） and 0.5-70 μg/L （r＝0.999 8）， respectively. The limits of quantitation were 0.003 1， 0.008 9， 0.016 0， 0.025 0， 0.002 1， 0.006 9， 0.038 1， 0.002 1， 0.005 5， 0.002 0， 0.023 1， 0.005 0， 0.002 0， 0.324 9 μg/L， separately. The limits of determination were 0.000 9， 0.002 7， 0.004 8， 0.007 5， 0.000 6， 0.002 1， 0.011 4， 0.000 6， 0.016 5， 0.000 6， 0.006 9， 0.001 5， 0.000 6， 0.097 5 μg/L， separately. RSDs of precision， stability and repeatability tests were all less than 8％. The recoveries were 87.4％-94.3％（RSD＝2.6％， n＝9）， 110.3％-118.2％（RSD＝1.8％，n＝9）， 89.8％-99.7％（RSD＝3.1％，n＝9）， 77.7％-84.4％（RSD＝2.5％，n＝9）， 105.6％-113.4％（RSD＝2.3％，n＝9）， 106.7％-116.5％（RSD＝2.7％，n＝9）， 89.1％-104.5％（RSD＝4.5％，n＝9）， 105.6％-118.6％（RSD＝3.6％，n＝9）， 77.8％-88.0％（RSD＝4.0％，n＝9）， 106.7％-116.1％（RSD＝2.8％，n＝9）， 88.5％-97.1％（RSD＝3.1％，n＝9）， 80.5％-88.6％（RSD＝2.9％，n＝9）， 85.2％-99.4％（RSD＝4.2％，n＝9）， 97.6％-109.3％（RSD＝3.2％，n＝9）， respectively. CONCLUSIONS： The method is simple， accurate. The precision， stability and repeatability of this method are also good. It is suitable for simultaneous determination of 14 elements in Deproteinized calf blood extractives injection.

Determination and risk assessment of heavy metals and harmful elements residues in Niuhuang Qingwei Pills based on ICP-MS / 中国中药杂志

To achieve a comprehensive understanding of heavy metals and harmful elements residues in Niuhuang Qingwei Pills,49 samples from 18 manufactures were collected from 31 provinces in China.Risk assessment and control preparations were applied innovatively in evaluation of exogenous pollution in traditional Chinese Medicine.Determination methods for Pb,Cd,As,Hg and Cu were established by inductively coupled plasma mass spectrometry(ICP-MS).Based on the procedures including hazard identification,hazard characterization,exposure assessment and risk characterization,risk assessment was performed and residual limits for Pb,Cd,As,Hg and Cu in the drug were formulated.The results showed that the hazardous quotients(HQ) of the elements were decreased in the following order:Pb>As>Cu>Hg>Cd,and the total hazardous index(HI) of heavy metals and harmful elements in Niuhuang Qingwei Pills was above 1,implying health risk of the drug.Under the proposed limits,5 elements in the control preparation as well as Cd and Cu in the samples were within the limits range,but the excess rates of Pb,As and Hg in the samples were 12%,12% and 14%,respectively.For the first time,basic steps for risk assessment of Chinese patent medicine were established,which provided model and reference for risk assessment and limit formulation of other drugs.

Determination of six arsenic species in traditional Chinese medicine Cordyceps by HPLC-ICP-MS / 国际药学研究杂志

Objective: To establish a high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS)method for the determination of trivalent arsenic(AsIII),pentavalent arsenic(As), methyl arsenic(MA),dimethyl arsenic(DMA),arsenical choline(AsC)and arsenical betaine(AsB)in traditional Chi- nese medicine Cordyceps. Methods: The arsenic species in Cordyceps were extracted with hot 0.15 mol/L nitric acid so- lution,separated by HPLC on a Dionex IonPacTM AS7 column(4 mm×250 mm,5 μm)with aqueous 5 mmol/L and 100 mmol/L ammonium carbonate solutions in a gradient elution as mobile phase,and quantitatively determined by ICP-MS. Results: The six kinds of arsenic species showed a good linearity within the range of 5-200 μg/kg. The average recovery was 83.3-115.9%,and the relative standard deviation was less than 5%. The main form of arsenic species in C ordyceps was inorganic arsenic(AsIIIand As),and the total content of ASIII+Asvaried around 1 mg/kg in the three tested batches of samples. Conclusion: The established HPLC-ICP-MS method is convenient,accurate and reliable for the analysis of different arsenic species in Cordyceps. In addition,the present work on the determination of six arsenic species in Cordy- ceps could be used as reference for improvement of the limitation standard of arsenic in Cordyceps.

Methodological validation: a method for determination of iodine in serum by inductively coupled plasma mass spectrometry / 中华地方病学杂志

Objective To validate a developing method for determination of iodine in serum by inductively coupled plasma mass spectrometry (ICP-MS).Methods Ammonium chloride,ethanolamine,ascorbic acid and water were mixed at a certain ratio,adding ethanol as sensitization,to dilute samples in the ratio of 1 ∶ 20,and then the diluted samples were analyzed by ICP-MS.Re was used as the internal standard.Serum samples were from 8 different individuals.After combining,they were divided into 4 groups,control group and low,medium and high iodine groups.Iodine groups were added with potassium iodide (100 mg/L),iodine standard solution 1.5,9.0,15.0 μl.The methodological evaluation of this method was done through standard curve linearity,sample detection limit,precision,recovery and accuracy in determining biological sample.And the results were compared with the current serum iodine arsenic cerium catalytic spectrophotometry standard method (WS/T 572-2017).Results The linear range of the calibration curve was 0-300 μg/L and the linear correlative coefficients of the standard curve were 0.999 8-1.000 0.The detection limit was 0.38 μg/L (the sample amount was 0.2 ml).The coefficients of variation (CV) were all below 2％ for 4 serum samples in precision.The recovery rate was in a range of 95.8％-108.5％.No significant difference was found between the results of the 15 serum samples determined by the standard method andthis new method (t =1.139,P ＞ 0.05).Conclusions The newly developed method in determination of iodine in serum by ICP-MS,has wide linear range,high sensitivity,good precision,and wide applicability.It is suitable for application in determining serum iodine.

Rapid determination of 21 elements in urine by inductively coupled plasma mass spectrometry / 中华劳动卫生职业病杂志

Objective@#To develop a rapid detection method for 21 elements in urine with inductively coupled plasma mass spectrometry (ICP-MS) .@*Methods@#The urine samples were directly diluted 20 times by 1% HNO3, and detected by ICP-MS, Indium, Yttrium, and Lutecium were used as on-line internal standard. Fe was analyzed by Dynamic Reaction Cell (DRC) mode, As, Cr, V and Zn were analyzed by collision cell technology (CCT) mode, and Be, Mn, Ni, Cd, Sn, Bi, Pb, Re, Sb, W, Li, Cu, Se, Sr, Mo were analyzed by standard mode. Dynamic band-pass tuning (DBT) was used to eliminate interference for Fe.@*Results@#All the elements have good linearity in their determination range, with the correlation coefficient r>0.999 5. The limits of detection of the 21 elements were in the range of 0.017-11.14 μg/L. The inter-precision (relative standard deviation, RSD) was less than 9.96%, and the intra-precision was less than 13.90% (except As RSD<18.91%) . The spike recovery of all elements fell within 81.1%-116.4%.@*Conclusion@#The method was proved to be simple, fast, and accurate, and met the needs of testing requirements of large amounts of specimens.

Determination of aluminum in blood of occupational workers by ICP-MS / 中华劳动卫生职业病杂志

Objective@#To establish a method for the determination of aluminum in blood, and to detect the aluminum content in the blood of occupational aluminum workers.@*Methods@#The morning blood of the aluminum workers was collected in an anticoagulation tube, and the supernatant was centrifuged. The supernatant was diluted with 4% nitric acid containing 1% Triton for 24 h at room temperature, and the supernatant was centrifuged. The supernatant was filtered and the blood aluminum concentration was measured by inductively coupled plasma mass spectrometry and quantified by external standard method.@*Results@#The detection limit of ICP-MS method was 0.39 μg/L, the linear range was 0-160 μg/L, the recoveries were 98.24%-99.65%, and the precision was 0.19%-0.28%. The recoveries of graphite furnace atomic absorption spectrophotometry (GFAAS) were 97.17%-111.18%, and the precision was 0.35%-0.44%. The average blood aluminum concentration of aluminum workers in the normal control group was (19.87±10.65) μg/L. The average blood aluminum concentration of aluminum workers in the expose group was (31.12±11.43) μg/L.@*Conclusion@#The method of ICP-MS for the determination of aluminum concentration in blood has a simple pretreatment process, high recovery rate, low detection limit and high precision, which is suitable for popularization.

Determination of serum iodine by inductively coupled plasma mass spectrometry / 中华地方病学杂志

Objective To determine serum iodine by inductively coupled plasma mass spectrometry (ICP-MS).Methods ICP-MS was used to determine iodine content directly by pretreatment method of diluting serum samples and standard series with diluent.The method was tested from correlation coefficient of standard curve,detection limit,precision,accuracy,etc.Results When the concentration of iodine in serum ranged from 0 to 300 μg/L,the linear correlation coefficient with the iodine ion counts determined by the instrument was 0.999 8 to 1.000 0 (n =6);the detection limit of iodine in serum was 1.24 μg/L;the relative standard deviation (RSD) ranged from 0.5％ to 1.5％ and from 0.3％ to 1.4％ for the intra-and inter-batch precision tests of seven different serum samples,respectively;the recovery rate of 7 serum samples with iodine content 40-230 μg/L ranged from 93.4％ to 109.2％,and the total average recovery rate was 102.4％.Conclusions Serum samples need not be pretreated before digestion,and can be directly injected after dilution with diluent without using highly toxic substances.The detection process is automatic,sensitive,precise,accurate and suitable for rapid quantitative determination of serum iodine content.