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ObjectiveTo obtain content characteristics of inorganic elements in Scutellariae Radix （aged 1-4 years）， and to explore the feasibility of identifying the growth years of Scutellariae Radix based on characteristic spectrum of inorganic elements combined with chemometric models. MethodAfter microwave digestion， the contents of Mn， Zn， Ca， Fe， Mg， Na， K， Cr， Cu， Se， As， Cd， Hg， Pb and Ni in 21 batches of Scutellariae Radix were determined by inductively coupled plasma atomic emission spectrometry （ICP-OES） and inductively coupled plasma mass spectrometry （ICP-MS）. Meanwhile， characteristic spectrum of inorganic elements in samples was drawn. The identification model was constructed to discriminate the growth years of Scutellariae Radix based on the combination of principal component analysis （PCA）， Fisher discriminant function and support vector machine （SVM）. ResultThe contents of Mn （7.79-36.48 μg·g-1）， Zn （10.12-31.43 μg·g-1）， Cu （6.38-17.20 μg·g-1）， K （2.98-13.89 μg·g-1）， Mg （3.45-7.78 μg·g-1） and Ca （2.32-7.09 μg·g-1） in Scutellariae Radix were detected by ICP-OES and ICP-MS， and their contents increased with the prolongation of growth years. PCA results showed that Cu， Ni， Cd， Na， Mg， Fe， Ca， Zn， Mn and Hg were characteristic elements of Scutellariae Radix. Samples with different years could be divided into four categories in the spatial characteristic diagram of Fisher discriminant analysis. The correct rate of SVM model for identifying the growth years of samples was 95.2%. ConclusionThis established method is accurate and rapid for discriminating the growth years of Scutellariae Radix， which can provide reference for the identification of other Chinese medicinal materials. It is suggested that some elements should be considered as indexes in subsequent construction of the quality evaluation system of Scutellariae Radix.
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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.
Subject(s)
Drugs, Chinese Herbal , Environmental Pollution/analysis , Mercury/toxicity , Metals, Heavy/toxicity , Risk AssessmentABSTRACT
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.
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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.
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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.
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China , Drug Contamination , Drugs, Chinese Herbal , Reference Standards , Metals, Heavy , Risk AssessmentABSTRACT
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.
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Objective@#The method was established for the detection of whole blood indium and serum indium. By comparing the results of two samples, it is possible to explore the significance of whole blood indium and serum indium in the population exposed to indium compounds.@*Methods@#According to GBZ/T 295-2017 and GBZ 294-2017, the whole blood and serum samples were diluted 20 times by 0.5% nitric acid solution (including 0.05% Triton X-100) . Under the standard mode of inductively coupled plasma mass spectrometry (ICP-MS) , whole blood indium and serum indium of indirect exposure group, low exposure group and high exposure group in an indium mine were detected with 20 μg/L rhodium standard solution as internal standard.@*Results@#This method has a working range of 0.00~5.00 μg/L and a correlation coefficien t>0.999. The detection limit and quantitative lower limit of whole blood indium were 0.076 μg/L and 0.26 μg/L respectively. Those of serum indium were 0.06 μg/L and 0.20 μg/L accordingly. The recovery rates of serum and whole blood samples were 88.5%~95.6% and 93.0%~101%. Intra batch precisions were 1.3%~4.4% and 1.9%~3.5% and inter batch precision were 2.4%~6.1% and 2.1%~4.6% in two samples. There were no significant differences between whole blood indium and serum indium in indirect exposure group. The serum indium level was lower than the detection limit in 3 cases, while their whole blood indium was only below the quantitative lower limit. However, in other groups whole blood indium level was significantly higher than serum indium level (P<0.05) and even was two-fold in the high exposure group.@*Conclusion@#The detection of whole blood indium is more sensitive than that of serum indium, which can reflect the internal exposure level more accurately in exposure population. Therefore, the whole blood indium is of more important referential value to health examination and poisoning diagnosis in the population exposed to indium and its compounds.
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@#Introduction: This study aims to quantify the concentrations of Cu, Cr, Zn, Ni, Pb, As and Cd in paddy soil and water and assess their potential dermal health risk to the farmers at Kampung Sawah Sempadan, Malaysia. Methods: 72 water samples and 72 soil samples were collected and analysed using inductively coupled plasma mass spectrometry (ICP-MS). 117 respondents were interviewed using a questionnaire to obtain the exposure information for dermal health risk assessments. Results: All elements in water did not exceed the recommended concentration by Malaysia National Water Quality Standard (NWQS) and Food and Agriculture Organization (FAO). Nevertheless, the maximum concentration of As (31.49 mg/kg) in paddy soil exceeded the Dutch Target Value for soil protection (29 mg/ kg). There was no significant chronic non-carcinogenic health risk for farmers working in the paddy soil and water (HQ<1, HI<1). The carcinogenic health risk of As was in the acceptable risk level (10-6 to 10-4). Conclusion: The contamination of the selected heavy metals in the paddy soil and water at Kampung Sawah Sempadan were lower than the available standards except for As in soil which exceeds the recommended value by Dutch target value. The health risk to these heavy metals were also minimal and within the acceptable level.
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Water QualityABSTRACT
Herbal-based slimming products which are consumed orally may be contaminated with heavy metals as well as microorganisms. This study aimed to evaluate the safety level of these slimming products by determining heavy metals and microbial contamination in different batch production. Six different brands of herbal-based slimming products (A, B, C, G, H and I) with three different batch productions (1, 2 and 3) were investigated (n =18). Five heavy metals Arsenic, Cadmium, Chromium, Copper and Zinc were determined using an Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). The presence of microorganisms was determined by total aerobic count and the bacteria were identified. The samples’ moisture content was determined by calculating the percentage of water loss after drying process. All batches of samples A and B had high content of zinc, over the permissible level of 5ppm while, 6 samples contained Chromium above the permissible level (1.5 ppm). All 3 batches of sample A presented with the highest total daily intake of heavy metals. Bacteria were present in all the samples tested with the highest numbers in samples G, H and A followed by B, I and C. The highest number of fungi was found in product A while product I was free from fungal contamination. Aspergillus spp. was the predominant fungus present in the samples. There was a weak correlation between moisture content and bacteria (r = 0.087) and fungal (r = 0.253) presence in the samples. As some herbal slimming products contain heavy metals as well as microorganisms, consumers need to be more vigilant and discerning when selecting products to be consumed.
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Metals, HeavyABSTRACT
Objective To establish a method of analyzing total uranium and 235U/238U ratio in urine using inductively coupled plasma mass spectrometry (ICP-MS) and uncertainty assessment.Methods Urine sample was digested with HNO3 and H2O2,and total uranium was determined using ICP-MS method directly.The digested urine sample was separated to concentrate uranium with tributyl phosphate (TBP) column,and 235U/238U ratio was analyzed using ICP-MS.The uncertainty was evaluated through sample pre-treatment,measurement and standard curve calculation.Results The recovery of total uranium in urine was 98.4％-102.4％,detection limit was 0.002 μg/L.The relative expanded uncertainty of total uranium concentration in urine was 0.26 (k =2).235 U/238 U ratio was 0.001 1 (k =2).Conclusions This study offers a low detection limit,good recovery and precision method for rapid determination of total uranium and 235U/238 U ratio in urine samples.It is potential used for both in occupational exposure assessment and nuclear emergency situation.The uncertainty evaluation of total uranium and 235U/238U ratio in urine are reliable.
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OBJECTIVE: To explore the dynamic changes of the inorganic elements in Polygoni Multiflori Radix.
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Objective To ascertain the uranium concentrations and uranium isotopic ratios in drinking water in Xilingol League,the Inner Mongolia Autonomous Region.Methods Drinking water samples were collected in Xilingol League,the Inner Mongolia Autonomous.Region inductively coupled plasma mass spectrometry (ICP-MS) was applied to determine the concentration of uranium and uranium isotope abundance.Results The uranium concentrations in all samples were in the range of 2.73-18.9μg/L,with an average of 8.20 μg/L.Tbe234U/238U isotope ratio varied from 7.513 × 10-5to 3.003 × 10-4 and235U/238U from 7.196 × 10-3 to 7.391 × 10-3.The relative standard deviation (RSD) was less than 0.5％ for234U/238U and 0.2％ for235 U/238U.Conclusions The uranium concentration in samples collected from Dongwuqi was high than 15 μg/L,whih is the limit given by World Health Organization (WHO).The uranium in drinking water originates from the natural environment.The234U is enriched in drinking water.