Association of blood heavy metal levels with osteocalcin abnormality and incidence of osteoporosis in Saudi subjects / Associação de anormalidades de osteocalcina nos níveis de metais pesados no sangue e incidência de osteoporose em indivíduos sauditas

Abstract Serum toxic metals have been implicated in development of many diseases. This study investigated the association between blood levels of lead and cadmium with abnormal bone mineral density (BMD) and incidence of osteoporosis. Sixty Saudi male adults age matching were assigned into two groups: A healthy control group (n = 30) and osteoporosis patients diagnosed according to T-score (n = 30). Serum calcium, vitamin D, osteocalcin, lead, cadmium were measured. Osteoporotic group showed a highly significant elevation of blood lead and cadmium levels compared to the control group (p <0.001). BMD was negatively correlated with serum osteocalcin level compared with control. There was a significant negative correlation between the cadmium and lead levels (r=-0.465 and p-value = 0.01) and calcium (p < 0.004). Our findings suggested that high cadmium and lead were negative correlated to BMD and increased the risk factor for osteoporosis.

Resumo Os metais tóxicos do soro têm sido implicados no desenvolvimento de muitas doenças. Este estudo investigou a associação entre os níveis sanguíneos de chumbo e cádmio com densidade mineral óssea anormal (DMO) e incidência de osteoporose. Sessenta adultos sauditas do sexo masculino com idades iguais foram divididos em dois grupos: um grupo de controle saudável (n = 30) e pacientes com osteoporose diagnosticados de acordo com o T-score (n = 30). Cálcio sérico, vitamina D, osteocalcina, chumbo, cádmio foram medidos. O grupo osteoporótico apresentou elevação altamente significativa dos níveis de chumbo e cádmio no sangue em comparação ao grupo controle (p < 0,001). A DMO foi negativamente correlacionada com o nível de osteocalcina sérica em comparação com o controle. Houve correlação negativa significativa entre os níveis de cádmio e chumbo (r = -0,465 ep = 0,01) e cálcio (p < 0,004). Nossos achados sugeriram que cádmio e chumbo elevados foram correlacionados negativamente à DMO e aumentaram o fator de risco para osteoporose.

Measurement of 239Pu in fecal samples based on inductively coupled plasma-mass spectrometry / 中国辐射卫生

Objective To establish a method for measurement of 239Pu in fecal samples based on inductively coupled plasma-mass spectrometry (ICP-MS), and to provide a novel method for assessing the internal exposure of workers. Methods Fecal samples were collected from workers and labeled. The samples were pretreated with carbonization ashing and microwave digestion devices, purified on TEVA resin, and measured using ICP-MS. Results The detection limit of 239Pu in fecal samples based on ICP-MS was 1.91 × 10−4 Bq. Conclusion In the routine monitoring of class S substances characterized by a 5 μm aerodynamic diameter during 12 months, the committed effective dose corresponding to the detection limit is 0.17 mSv. This value meets the requirements of relevant national standards and ICP-MS can be used as a novel means for accurate evaluation of internal exposure for workers.

Determination uncertainty of aluminum residues in human albumin using top-down evaluation / 中国输血杂志

【Objective】 To evaluate the determination uncertainty of aluminum residues in human albumin by inductively coupled plasma mass spectrometry (ICP-MS). 【Methods】 The aluminum residues in human albumin was determined by ICP-MS, and the top-down method was applied to assess the reasons of uncertainty and calculate the uncertainty. 【Results】 The relative standard uncertainty of the aluminum content in human albumin at the three quality control levels was 0.54 ng/mL, 1.68 ng/mL and 4.54 ng/mL, respectively, which met the requirements of the guidelines for bioanalytical methods in the Chinese Pharmacopoeia(2020). 【Conclusion】 The top-down method is simple and quick to assess the uncertainty of aluminum residues in human albumin, and is suitable for the uncertainty assessment of analytical methods in biological laboratories.

Association of blood heavy metal levels with osteocalcin abnormality and incidence of osteoporosis in Saudi subjects / Associação de anormalidades de osteocalcina nos níveis de metais pesados no sangue e incidência de osteoporose em indivíduos sauditas

Serum toxic metals have been implicated in development of many diseases. This study investigated the association between blood levels of lead and cadmium with abnormal bone mineral density (BMD) and incidence of osteoporosis. Sixty Saudi male adults age matching were assigned into two groups: A healthy control group (n = 30) and osteoporosis patients diagnosed according to T-score (n = 30). Serum calcium, vitamin D, osteocalcin, lead, cadmium were measured. Osteoporotic group showed a highly significant elevation of blood lead and cadmium levels compared to the control group (p <0.001). BMD was negatively correlated with serum osteocalcin level compared with control. There was a significant negative correlation between the cadmium and lead levels (r=-0.465 and p-value = 0.01) and calcium (p < 0.004). Our findings suggested that high cadmium and lead were negative correlated to BMD and increased the risk factor for osteoporosis.

Os metais tóxicos do soro têm sido implicados no desenvolvimento de muitas doenças. Este estudo investigou a associação entre os níveis sanguíneos de chumbo e cádmio com densidade mineral óssea anormal (DMO) e incidência de osteoporose. Sessenta adultos sauditas do sexo masculino com idades iguais foram divididos em dois grupos: um grupo de controle saudável (n = 30) e pacientes com osteoporose diagnosticados de acordo com o T-score (n = 30). Cálcio sérico, vitamina D, osteocalcina, chumbo, cádmio foram medidos. O grupo osteoporótico apresentou elevação altamente significativa dos níveis de chumbo e cádmio no sangue em comparação ao grupo controle (p < 0,001). A DMO foi negativamente correlacionada com o nível de osteocalcina sérica em comparação com o controle. Houve correlação negativa significativa entre os níveis de cádmio e chumbo (r = -0,465 ep = 0,01) e cálcio (p < 0,004). Nossos achados sugeriram que cádmio e chumbo elevados foram correlacionados negativamente à DMO e aumentaram o fator de risco para osteoporose.

Association of blood heavy metal levels with osteocalcin abnormality and incidence of osteoporosis in Saudi subjects

Abstract Serum toxic metals have been implicated in development of many diseases. This study investigated the association between blood levels of lead and cadmium with abnormal bone mineral density (BMD) and incidence of osteoporosis. Sixty Saudi male adults age matching were assigned into two groups: A healthy control group (n = 30) and osteoporosis patients diagnosed according to T-score (n = 30). Serum calcium, vitamin D, osteocalcin, lead, cadmium were measured. Osteoporotic group showed a highly significant elevation of blood lead and cadmium levels compared to the control group (p 0.001). BMD was negatively correlated with serum osteocalcin level compared with control. There was a significant negative correlation between the cadmium and lead levels (r=-0.465 and p-value = 0.01) and calcium (p 0.004). Our findings suggested that high cadmium and lead were negative correlated to BMD and increased the risk factor for osteoporosis.

Resumo Os metais tóxicos do soro têm sido implicados no desenvolvimento de muitas doenças. Este estudo investigou a associação entre os níveis sanguíneos de chumbo e cádmio com densidade mineral óssea anormal (DMO) e incidência de osteoporose. Sessenta adultos sauditas do sexo masculino com idades iguais foram divididos em dois grupos: um grupo de controle saudável (n = 30) e pacientes com osteoporose diagnosticados de acordo com o T-score (n = 30). Cálcio sérico, vitamina D, osteocalcina, chumbo, cádmio foram medidos. O grupo osteoporótico apresentou elevação altamente significativa dos níveis de chumbo e cádmio no sangue em comparação ao grupo controle (p 0,001). A DMO foi negativamente correlacionada com o nível de osteocalcina sérica em comparação com o controle. Houve correlação negativa significativa entre os níveis de cádmio e chumbo (r = -0,465 ep = 0,01) e cálcio (p 0,004). Nossos achados sugeriram que cádmio e chumbo elevados foram correlacionados negativamente à DMO e aumentaram o fator de risco para osteoporose.

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.

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.

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.

Exploration of ²⁴¹Am measurement in fecal samples / 中国辐射卫生

@#<b>Objective</b> To preliminarily study and establish a method for measurement of the transuranic nuclide ²⁴¹Am in fecal samples, and to provide technical support for internal radiation monitoring of staff. <b>Methods</b> Fecal samples were collected with a self-made stool sampler and treated with a self-made carbonization and ashing furnace. DGA resin was used to separate and purify ²⁴¹Am from fecal samples. With ²⁴³Am as the tracer, the orthogonal method was used for condition optimization. <b>Results</b> The optimum conditions for separation and purification were: the acidity of HNO₃ added into the column, 6 mol/L; column flow rate, 0.6 mL/min; and the volume of analytical solution,12 mL. The method based on inductively coupled plasma mass spectrometry showed a detection limit of 9.79×10⁻⁴ Bq for ²⁴¹Am in fecal samples, which was satisfactory and feasible. <b>Conclusion</b> This method fills the vacancy of ²⁴¹Am measurement in fecal samples to some extent, which is of practical significance for internal radiation monitoring and protection for analysts.

Analyzing the difference between atomic fluorescence spectrometry and ICP-MS in the determination of arsenic in urine / 中国职业医学

@#Abstract: Objective （ ） To compare the measured results of arsenic in urine by atomic fluorescence spectrometry AFS and - （ - ）， Methods inductively coupled plasma mass spectroscopy ICP MS and analyze the reasons of the difference. The samples WS/T 474-2015 Determination of Arsenic in Urine by Hydride Generation Atomic Fluorescence were pretreated according to Spectrometry， （ ∶ ∶ ∶∶ ，V/V/V） and digested with mixed acid nitric acid sulfuric acid perchloric acid=3 1 1 and then determined by - - AFS and ICP MS. The samples were diluted with 0.50% nitric acid and determined by ICP MS. The samples included urine ， ， （ arsenic quality control samples inorganic arsenic supplemented samples and organic arsenic arsenic choline and arsenic ） - betaine supplemented samples. Standard curve method was used to compare the results of AFS method and ICP MS method. Results （ ） （ ） The results of quality control samples by AFS method digestion and ICP-MS method without digestion were ， - within the range of reference values but the values obtained by AFS method were lower than those obtained by ICP MS method. - - - ， The recovery of AFS and ICP MS was 97.79% 100.82% and 99.55% 99.98% respectively. In the middle and high ， - （ P ） concentration groups the measured values of inorganic arsenic by AFS were lower than that by ICP MS all <0.01 . The （ ） - recovery of arsenic betaine and arsenic choline by AFS method digestion was only 2.17% 2.63%. The values of arsenic betaine （ ） - （ and arsenic choline measured by AFS method digestion were lower than those measured by ICP MS method without ） - （ ）（ P ）Conclusion digestion and ICP MS method digestion all <0.01 . The result of urine arsenic measured by AFS method - ， was lower than that measured by ICP MS method which may be related to the mixed acid digestion of AFS method. Keywords: ； - ； ； ； ； ；

Evaluation of uncertainty for the determination of lead in ambient air PM2.5 by ICP-MS / 公共卫生与预防医学

Objective To establish an evaluation method of uncertainty for the determination of lead in ambient air PM2.5 by inductively coupled plasma mass spectrometry (ICP-MS). Methods According to HJ657-2013 “Determination of Lead and Other Metal Elements in Air and Exhaust Particulates by Inductively Coupled Plasma Mass Spectrometry”, the concentration of lead in ambient air PM2.5 was determined. A mathematical model was established to analyze the source of uncertainty and to calculate each component of uncertainty. The components were combined into the standard uncertainty, and the relative expanded uncertainty was finally obtained. Results The expanded uncertainty of lead in ambient air PM2.5 was 0.16 ng/m3, and the measurement result of lead was (1.75±0.16)ng/m3. Conclusion The main source of uncertainty of this method comes from the relative standard uncertainty introduced by sample pretreatment.

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.

Content Determination of 20 Element Impurities in Aminomethylbenzoic Acid Injections and Its Compatibility Investigation / 中国药房

OBJECTIVE：To establish a m ethod to determine the cont ents of 20 elements impurities in Aminomethylbenzoic acid injection ，and to investigate its compatibility in low-borosilicate glass ampoules. METHODS ：The sample was diluted with 5％ nitric acid solution ，and then determined by ICP-MS using scandium ，indium and bismuth as internal standards. The nebulizer flow（argon）was 0.92 L/min，collision gas flow （helium）was 4.5 L/min，RF power was 1 895 W，plasma flow was 18 L/min， pump speed was 40 r/min，injection delay time was 65 s. The collision mode was used as measurement mode ，the data sampling adopted peak skipping mode ，and repeated for 3 times. The accelerated test was carried out after sample was stored at 70 ℃ for 1 and 3 months，and the compatibility was investigated by comparing the change trend of element impurity content. RESULTS ：The linear range of vanadium ，cobalt，chromium，arsenic，cadmium，antimony，mercury，thallium and lead were 0.01-20 μg/L；those of magnesium ，aluminium，ferrum，nickel，copper，zinc，barium were 0.1-200 μg/L；those of boron ，silicon，potassium and calcium were 1-2 000 μg/L（r≥0.999 8）. RSDs of precision ，intermediate precision ，stability（8 h）and repeatability test were all lower than 6％. The limits of quantitation were 0.000 7-2.986 3 μg/L；the limits of detection were 0.000 2-0.895 9 μg/L. The average recoveries were 88.50％-111.00％（RSDs were 0.52％-2.33％，n＝9）. The minimum content of 20 element impurities was less than detection limits ，the maximum contents were 3 835.9 μg/L（0 month），10 448.4 μg/L（1 month），17 261.2 μg/L（3 month） in Aminomethylbenzoic acid injection from 8 manufacturers. Among the 20 elements impurities ，except that boron ， aluminum，magnesium，silicon，calcium and potassium were not specified ，the contents of other elements were less than the threshold. The research of compatibility showed that the impurity contents of seven elements such as boron ，aluminum，silicon， potassium，zinc，arsenic and barium showed an increasing trend. The silicon concentration ，silicon/aluminum concentration ratio and silicon/boron concentration ratio in the accelerated samples after stored for one and three months were significantly different from those stored for 0 month. CONCLUSIONS ：The established method is sensitive ，reproducible and accurate ，and can be used for the content determination of 20 element impurities in Aminomethylbenzoic acid injection. The interaction between low-borosilicate ampoule and Aminomethylbenzoic acid injection is obvious.

Comparison of the Contents of 14 Inorganic Elements in Cyperus rotundus from Different Origins Based on Stoichiometry / 中国药房

OBJECTIVE：To establish the method for the content determination of inorganic elements in Cyperus rotundus ，and to compare the contents of 14 kinds of inorganic elements in C. rotundus from different producing areas ，and to provide theoretical basis for its quality control and high quality resources development . METHODS ：The samples were processed by microwave digestion，and ICP-MS method was used to determine the contents of Na ，Mg，K，Ca，Mn，Fe，Ni，Cu，Zn，As，Se，Sr，Cd and Pb. SPSS 23.0 software were used for principal component analysis （PCA）and cluster analysis. RESULTS ：The average contents of above 14 kinds of inorganic elements in C. rotundus from different producing areas were 168.62，753.71， 6 938.33，24.31，14.69，197.77，0.60，2.43，26.89，0.21，0.06，5.64，0.05，0.32 mg/kg，respectively. The results of PCA showed that the cumulative variance contribution rate of the first four principal components was 86.203％，which could reflect most of the information of the original data. C. rotundus from Shandong ，Jiangxi，Shanxi，Hubei and Yunnan ranked the top five places in terms of comprehensive score of inorganic element contents. The results of cluster analysis showed that the samples from 9 producing areas were clustered into 5 categories，showing the characteristics of clustering by producing area. From the perspective of inorganic elements ，the quality of C. rotundus from East China ，Central China ，North China and Southwest China was better than that from South China. CONCLUSIONS ：Essential trace elements like Na ，Mg，K，Ca，Mn，Fe，Cu，Zn，Sr are rich in C. rotundus，and there are small amounts of Ni ，As，Se，Cd，Pb elements in it. The contents difference of inorganic elements in C. rotundus from different origins may related to the geographical area it belongs to.

Content Analysis of 5 Kinds of Heavy Metal in Yougui Pills / 中国药房

OBJECTIVE：To investigate the contents of 5 kinds of heavy metal as copper （Cu），arsenic（As），cadmium （Cd），mercury（Hg）and lead （Pb）in Yougui pills ，and to evaluate its safety risk. METHODS ：Using yttrium （89Y），indium （115In）and bismuth （209bi）as internal standard ，the contents of each element were determined by ICP-MS. ICP-MS condition included that atomization gas flow rate was 0.95 L/min，auxiliary gas flow rate was 1.2 L/min，plasma gas （argon）flow rate was 18 L/min，pump speed was 30 r/min. RF power of inductively coupled plasma was 1 200 W，the voltage in simulation stage was 1 750 V，the voltage in pulse stage was 1 300 V，the voltage of deflection device was －12 V，and the detector was in analog and pulse dual-mode. The determination methods of various elements were investigated ，and 45 batches of marketed Yougui pills were determined. Hazard index （HI）was used to analyze the non-carcinogenic risk of each element and calculate the maximum residual limit（MRL）of each element. RESULTS ：The linear range of Cu ，As，Cd，Hg and Pb ranged from 10-200，1-50，0.4-30，0.2-6 and 2-100 μg/L（all r＞0.999 0），respectively. The limits of quantitation were 0.67，0.23，0.20，0.07，0.27 μg/L. The limits of detection were 0.20，0.07，0.06，0.02，0.08 μg/L. RSDs of precision，stability and reproducibility tests were all lower than 3.5％ （n＝6 or n＝5）. Average recoveries were 92.96％-100.89％（RSD＝2.23％-3.62％，n＝3）. Average contents of Cu ，As，Cd，Hg and Pb in 45 batches of Yougui pills were 2.72，0.28，0.07，0.05，0.62 mg/kg，and superimposed HI of each element was less than 1. The contents of 5 kinds of heavy metals in Yougui pills were lower than the proposed MRL （MRL of Cu ，As，Cd，Hg and Pb were 20，2，1，0.2，5 mg/kg or 111.11，4.44，2.22，1.48，8.89 mg/kg respectively ）. CONCLUSIONS ：Established method can be used for the determination of content of 5 kinds of heavy metal in Yougui pills ；the heavy metal pollution rate of marketed Yougui pills is low and the safety risk is small.

Determination of the Contents of Heavy Metals and Harmful Elements in Pediatric ，Paracetamol，Atificial Cow- bezoar and Chlorphenamine Maleate Granules by ICP-MS / 中国药房

OBJECTIVE：To es tablish a method for the content determination of heavy metals [lead （Pb），cadmium（Cd）， copper （Cu）， mercury （Hg）] and harmful elements [arsenic （As）] in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules. METHODS ：The samples were conducted pretreatment by microwave digestion instrument and determined by inductively coupled plasma mass spectrometry （ICP-MS）using elements germanium ，indium，bismuth as internal standard. RESULTS ：The linear ranges of Pb ，As，Cu，Cd and Hg were 1-20，0.5-10，5-100，0.5-10 and 0.2-4 ng/mL， respectively （all r＞0.997）. The limits of detection （LODs） were 0.041 1，0.013 2，0.057 3，0.009 0，0.005 4 ng/mL， respectively. The limits of quantification （LOQs）were 0.137 0，0.044 0，0.191 0，0.030 0，0.018 0 ng/mL，respectively. RSDs of precision and repeatability tests were all less than 6％. RSDs of stability tests （28 h）of Pb ，As，Cu and Cd were all less than 5％， and that of stability test （28 h）of Hg was less than 7％. The average recoveries were 89.44％（RSD＝5.87％，n＝9），99.56％ （RSD＝5.46％ ，n＝9），96.12％（RSD＝4.62％ ，n＝9），105.82％（RSD＝2.80％ ，n＝9）and 90.23％（RSD＝3.59％ ，n＝9）， respectively. Five elements were all detected in 63 batches of samples ，and the contents of them were 0.191 0-1.527 6，0.002 5- 0.047 4，0.034 1-1.549 0，0.001 5-0.078 8 and 0.001 9-0.005 4 mg/kg，respectively. CONCLUSIONS ：The method is simple ， sensitive and accurate. It is suitable for simultaneous determination of 5 elements in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules.

Phenolic compounds, biological activities and trace elements of Capparis ovata var. canescens

Introduction: Capparis species (Capparaceae), also called caper, grow naturally in various regions of the world. Caper is a plant with medicinal and aromatic properties. Flower buds, root bark, and fruits of the plant areused in folk medicine due to their analgesic, wound healing,cell regeneration, tonic, and diuretic effects. Objective: The aim of this research was to evaluate in vitro (anti-urease, antioxidant, anticholinesterase) and in vivo (anti-inflammatory) biological activities of caper (C. ovatavar.canescens). In addition, we aimed to identify its major phenolic compounds using high performance liquid chromatography with a photodiode array detector (HPLC-DAD) and confirmate them using quadrupole time-of-flight liquid chromatography with tandem mass spectrometry (Q-TOF-LC/MS). Also, we quantified the concentrations of several trace and major elements in plant samples using inductively coupled plasma-mass spectrometry (ICP-MS). Methods: The antioxidant, anti-urease and anticholinesterase activities of different plant extracts were evaluated using DPPH, FRAP, ABTS/TEAC, Indophenol and Ellman tests. The identification of phenolic compounds and trace element contents was performed using HPLC and Q-TOF-LC/MS and ICP-MS. Results: Soxhlet methanol extract exhibited the strongest anti-urease, antioxidant (ABTS/TEAC) and anticholinesterase activity. Soxhlet and maceration methanol extracts demonstrated significant anti-inflammatory effect in the altered edema size after the second hour of carrageenan injection. The active phenolic compounds in Soxhlet methanol extract were identified as rutin, quercetin-hexoside-hexoside, quercetin-3-O-hexoside and kaempferol-3-O-rutinoside. In addition, the average concentrations of vanadium, chromium, manganese, cobalt, copper, nickel, arsenic, selenium, zinc and lead were within the permissible limits defined by WHO for medicinal plants. However, it was found that the concentrations of cadmium and iron were higher than the maximum permissible limits. Conclusion: Our results suggest that although caper has a strong biological activity, it should be consumed carefully due to the excess amount of cadmium and iron elements it contains.

Introducción: Las especies de Capparis (Capparaceae), también llamadas alcaparras, crecen naturalmente en varias regiones del mundo. La alcaparra es una planta con propiedades medicinales y aromáticas. Los botones florales, la corteza de la raíz y los frutos de la planta se usan en la medicina popular debido a sus efectos analgésicos, cicatrizantes, de regeneración celular, tónicos y diuréticos. Objetivo: El objetivo de esta investigación fue evaluar las actividades biológicas in vitro (anti-ureasa, antioxidante, anticolinesterasa) e in vivo (antiinflamatorio) de la alcaparra (C. ovata var. canescens). Además, nuestro objetivo fue identificar sus principales compuestos fenólicos mediante cromatografía líquida de alto rendimiento con un detector de matriz de fotodiodos (HPLC-DAD) y confirmarlos mediante cromatografía líquida con espectrometría de masas en tándem (Q-TOF-LC/MS). Además, cuantificamos las concentraciones de varios elementos traza y elementos mayores en muestras de la planta utilizando espectrometría de masas con plasma acoplado inductivamente (ICP-MS). Métodos: Se evaluaron las actividades antioxidantes, anti-ureasa y anticolinesterasa de diferentes extractos de la planta usando las pruebas DPPH, FRAP, ABTS/TEAC, Indofenol y Ellman. La identificación de los compuestos fenólicos y el contenido de los elementos traza se realizó mediante HPLC y Q-TOF-LC/MS e ICP-MS. Resultados: El extracto de metanol Soxhlet exhibió la mayor actividad anti-ureasa, antioxidante (ABTS/TEAC) y anticolinesterasa. Los extractos de metanol Soxhlet y por maceración demostraron un efecto antiinflamatorio significativo en el tamaño alterado del edema después de la segunda hora de la inyección de carragenano. Los compuestos fenólicos activos en el extracto de metanol Soxhlet se identificaron como rutina, quercetina-hexósido-hexósido, quercetina-3-O-hexósido y kaempferol-3-O-rutinósido. Además, las concentraciones promedio de vanadio, cromo, manganeso, cobalto, cobre, níquel, arsénico, selenio, zinc y plomo estaban dentro de los límites permisibles definidos por la OMS para las plantas medicinales. Sin embargo, se encontró que las concentraciones de cadmio y hierro fueron más altas que los límites máximos permitidos. Conclusión: Nuestros resultados sugieren que, aunque la alcaparra tiene una fuerte actividad biológica, debe consumirse con cuidado debido al exceso de cadmio y hierro que contiene.

Study on difference of chemical compositions of Guilingji before and after alchemy based on mass spectrometry and multivariate statistical analysis / 中国中药杂志

UPLC-Q-Orbitrap MS/MS and ICP-MS coupled with multivariate statistical analysis was employed to explore the differences in chemical compositions of Guilingji(GLJ) before and after alchemy.The changes in organic chemical compositions and inorganic elements were observed and 39 differential organic compositions were found in GLJ after alchemy, 24 compounds of which were identified. The differential compositions of GLJ included violet ketones, chalcones, amides, and fatty acids whose contents were increased after alchemy, as well as flavones, isoflavones, dihydroflavones, flavonoid glycosides, and coumarins whose content were decreased after alchemy. This study showed 6 inorganic elements filtered out as markers for distinguishing GLJ before and after alchemy, including B, Si, Mg, K, Cr, and Ni.The contents of Mg, K, Cr and Ni were increased while the contents of B and Si were decreased after alchemy.The difference of the contents after alchemy changed the cold and hot properties of the compound, showing the decrease of dryness, and the hot property was changed to warm and neutral properties; in addition, the membrane permeability and absorption of the compound compositions were improved. In this study, we preliminarily investigated the changes of chemical compositions in GLJ before and after alchemy as well as the effects of alchemy on physical and chemical properties and cold-heat nature of GLJ, laying a foundation for further clarifying the scientific connotation of alchemy process.

Determination of heavy metal contents in Gardeniae Fructus and fried Gardeniae Fructus and their health risk assessment / 中国中药杂志

In this study, the contents of Cu, As, Cd, Pb and Hg in 10 batches of Gardeniae Fructus and 10 batches of fried Gardeniae Fructus from Fuzhou in Jiangxi were determined by inductively coupled plasma mass spectrometry(ICP-MS), and the target hazard coefficient(THQ) for different drug users(adults and children) was calculated by using the international health risk assessment model. According to the ISO and green industry standard, the content of Hg in 4 batches of Gardeniae Fructus exceeded the standard with an over-standard rate of 40%. The THQ and total THQ of Hg in 2 batches of Gardeniae Fructus were higher than the international standard limit of Gardeniae Fructus. For 10 batches of fried Gardeniae Fructus, the content of every heavy metal and total amount of five heavy metals did not exceed the standard. However, the THQ and total THQ of Hg in 1 batch of fried Gardeniae Fructus were higher than the international standard limit of Gardeniae Fructus. As compared with Gardeniae Fructus, the contents of Cu, Pb and Hg in fried Gardeniae Fructus decreased by 34.0%, 77.6% and 23.1%; the THQ of Cu, Pb and Hg for adults decreased by 33.3%, 75.0% and 96.9%; and the THQ of Cu, Pb and Hg for children decreased by 37.5%, 75.0%, 90.7%. It showed that the contents of heavy metals in individual batches of Gardeniae Fructus in this experiment had a certain risk to human health, but the contents of these heavy metals in fried Gardeniae Fructus had no obvious effect on human health. This study provided experimental basis and research ideas for safety evaluation of Gardeniae Fructus and fried Gardeniae Fructus.

Evaluation of Erythrocyte Iron Incorporation in Beijing Prepubertal Children Using a Single Stable Isotope Tracer Method / 生物医学与环境科学（英文）

Objective@#To analyze the rate of erythrocyte iron incorporation and provided guidance for the iron nutrition for prepubertal children.@*Methods@#Fifty-seven prepubertal children of Beijing were involved in this study and each subject was orally administered 3 mg of Fe twice daily to obtain a total of 30 mg Fe after a 5-d period. The stable isotope ratios in RBCs were determined in 14th day, 28th day, 60th day, and 90th day. The erythrocyte incorporation rate in children was calculated using the stable isotope ratios, blood volume and body iron mass.@*Results@#The percentage of erythrocyte Fe incorporation increased starting 14 th day, reached a peak at 60 d (boys: 19.67% ± 0.56%, girls: 21.33% ± 0.59%) and then decreased. The erythrocyte incorporation rates of Fe obtained for girls in 60th day was significantly higher than those obtained for boys ( < 0.0001).@*Conclusions@#The oral administration of Fe to children can be used to obtain erythrocyte iron incorporation within 90 d. Prepubertal girls should begin to increase the intake of iron and further studies should pay more attention to the iron status in prepubertal children.