Marine sediments were dissolved by HNO3-HF-HC104 in a sealed container at low pressure; HF was evaporated in an open container and salts were dissolved in HCl by heating, then transferred to 2% HNO3 solution. A total ...Marine sediments were dissolved by HNO3-HF-HC104 in a sealed container at low pressure; HF was evaporated in an open container and salts were dissolved in HCl by heating, then transferred to 2% HNO3 solution. A total of 45 elements, including Li, Be, Sc, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Cd, In, Sb, Cs, Ba, La, Ce, Pr, Nd, Sin, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Tl, Pb, Bi, Th and U, were measured by inductively coupled plasma mass spectrometry （ICP-MS）. Conditions and sample experiments showed that this procedure defines a good experimental method which has the advantages of clear interference, easy operation and reliable results. The concentrations of the 45 elements could be used for resource exploration, environmental assessment and academic research.展开更多
Raohe honey (Honey in Raohe) is the only product which has obtained China’s national geographical mark for honey;however, it is always counterfeited by some producers due to its excellent quality. In this research, R...Raohe honey (Honey in Raohe) is the only product which has obtained China’s national geographical mark for honey;however, it is always counterfeited by some producers due to its excellent quality. In this research, Raohe honey was identified by geographical sourcing, where the detection on 166 Raohe honey samples and 31 non-Raohe honey samples was conducted with Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Additionally, the method of Primary Composite Analysis accomplished dimensionality reduction by transforming the abundance ratios variables of 13 isotopes to 4 primary composites, and could explain 91.17% of the total variables. There were five models: Decision Tree, Naive Bayes, Neural Network, Partial Least Square Discriminate and Support Vector Machine, built on the four new variables of primary composites with the Agilent MPP Software. The validation of the models was performed with 11 Raohe honey samples and 5 non-Raohe honey samples randomly selected. The accuracies of the Decision Tree and Support Vector Machine models were both 93.97%, and those of the Naive Bayes and Neural Network models were both 87.5%, while the contribution rate of the Partial Least Square Discriminate model was only 75%. It was concluded that the Decision Tree and Support Vector Machine models could be used for indentifying Raohe honey, and the Naive Bayes and Neural Network models could work as references, while the Partial Least Square Discriminate model was not suitable for identifying Raohe honey.展开更多
Individual monitoring of workers exposed to the risk of intake of actinides requires suitable methods for measuring low level of excreted activity. The current protocols used for actinides analysis in bioassay are usu...Individual monitoring of workers exposed to the risk of intake of actinides requires suitable methods for measuring low level of excreted activity. The current protocols used for actinides analysis in bioassay are usually complicated and highly time consuming. In this work, a protocol based on the microwave digestion of urines followed by the separation of actinides using calix[6]arene-based chromatography columns and their measurement by a quadrupole ICP-MS is developed and validated, for the first time, on urine samples containing the three actinides, U, Pu and Am. With this protocol, the total analysis time is about 2 days, including the mineralization of urine and the chromatographic separation of actinides. Detection limits of actinides in urine are determined and compared to those obtained after “dilute and shoot” ICP-MS analysis or after alpha spectrometry measurement.展开更多
[Objectives]To detect content of Pb,Cd,Hg,As,Cu,Zn,and Cr in Lysimachia christinae,and to analyze the pollution level.[Methods]Seven kinds of elements in L.christinae were determined by Inductively coupled plasma mass...[Objectives]To detect content of Pb,Cd,Hg,As,Cu,Zn,and Cr in Lysimachia christinae,and to analyze the pollution level.[Methods]Seven kinds of elements in L.christinae were determined by Inductively coupled plasma mass spectrometry and analyzed by single index and comprehensive index.[Results]The seven heavy metal elements showed good linearity in their respective concentration ranges.The recoveries of the samples were 84.5%-109.5%,and the RSD values were 2.30%-5.10%.Comparing the measured results of heavy metal elements with the limit values stipulated in the 2020 edition of the Chinese Pharmacopoeia and other standards,the Cr element in 19 batches of samples exceeded the standard,and the Zn element in 7 batches of samples exceeded the standard.The exceeding rates were 100.0%and 36.8%,respectively;the content of other heavy metal elements did not exceed the standard.The order of individual index from large to small was Cr,Zn,Cd,Hg,Cu,As,and Pb,and the average comprehensive pollution level was mild pollution and above.[Conclusions]L.christinae was mainly polluted by Cr,followed by Zn;this study can provide basic data for drafting of the limit standard for heavy metal elements in L.christinae.展开更多
A quick and sensitive method was developed for the determination of 19 metal elements in Saffron,a traditional Chinese medicinal herb,collected from Tibet Autonomous Region and Henan Province of China using inductivel...A quick and sensitive method was developed for the determination of 19 metal elements in Saffron,a traditional Chinese medicinal herb,collected from Tibet Autonomous Region and Henan Province of China using inductively coupled plasma atomic emission spectrometry（ICP-AES）or inductively coupled plasma mass spectrometry（ICP-MS）.The determined 19 metals in Saffron include Ca,Fe,Mg,P,Sr,Al,Mn,Zn,V,Cr,Se,Co,Ni,Mo,and heavy metals As,Cu,Cd,Hg and Pb.For all the analyzed elements,the correlative coefficients of the calibration curves were no less than 0.9938.This proposed method was accurate,and the relative standard deviations of the measurements were lower than 5.25%.It can be used for the quality control of metal elements in Saffron.展开更多
Thiols play vital roles in cellular metabolism knowledge of which may be important in the design of future anticancer drugs. Previous work on the composition of the thiols present in human cancer cell lines has shown ...Thiols play vital roles in cellular metabolism knowledge of which may be important in the design of future anticancer drugs. Previous work on the composition of the thiols present in human cancer cell lines has shown the presence of an unknown low molecular weight species, deemed to be a “Conthiol”, which could be important in this respect. This was prepared and isolated from a human prostate cancer cell line (LNCaP) in the form of an adduct of 2-mercuri-4-nitrophenol;it accounts for 56.5% of the total cellular thiols present in this cell line. Initial LC-MS analysis of this adduct had indicated that the possible molecular weight of the thiol was in the region of 467 daltons. In further analytical studies to identify the thiol, attempts were made to release it from the adduct by passage through a Thiopropyl Sepharose6B column. LC-MS analysis of the column eluate revealed two components yielding negative ion fragments of 427 m/z and 449 m/z. Only the former component contained thiol, indicating that a breakdown and/or possible rearrangement of the Conthiol had occurred. Further investigations of the column thiol eluate using ICP-MS analysis showed that the sulfur content agreed with the spectrophotometric analysis result (Ellman assay) and that the molecule did not contain phosphate. Amino acid analyses of the eluate were negative. In an attempt to prevent the breakdown of the thiol released by the Thiopropyl Sepharose 6B column, the adduct was treated with 5% v/v bromine water prior to applying to the column. In this instance the thiol containing eluate obtained from the column was treated with an equimolar quantity of mercuric chloride forming a fresh adduct, RS-Hg-SR. LC-MS analysis of this mercurial adduct detected a negative ion fragment of 782 m/z which on further ionization gave a ladder like pattern showing loss of mass units of 58 in each rung. This would seem to suggest the presence of a repeat polymer like structure containing 5 monomers, which, plus the thiol atom, gives a possible formula weight of 322;probably revealing only a part of the unknown Conthiol molecule whose properties and formula weight do not correlate with any known cellular thiol. Further analysis of the thiol released from the adduct on the Thiopropyl Sepharose 6B column by Infra-red (FTIR) provided little information except to confirm the presence of the thiol group and C=O stretch bands together with the possibility of a lactam ring at 1651 and 1634 cm·s<sup>-</sup><sup>1</sup>.展开更多
At the beginning of rare earth industry,several days are normally required for characterization of rare earth elements(REEs)fractionation in ore samples.Herein,rapid fractionation analysis of 15 REEs and accompanied m...At the beginning of rare earth industry,several days are normally required for characterization of rare earth elements(REEs)fractionation in ore samples.Herein,rapid fractionation analysis of 15 REEs and accompanied metal(Fe,Mn,etc.)in ore samples has been achieved within 1 h using ICP-MS with a homemade device for online sequential solvent extraction.As a result,five fractionations for REEs occurrences,i.e.,water soluble,exchangeable,reducible,oxidizable and crystalline,have been identified,offering chemical insights which not only reveal the formation mechanism of REEs ores but also show great implications for guiding the exploitation and separation of REEs.In comparison with conventional methods,the present approach significantly shortened the analysis time(1 h vs.~80 h)and reduced the sample consumption(1.0 mg vs.5.0 g)with high recovery(>95%),providing a useful platform for the rapid quantitative fractionation analysis of REEs in complexed samples such as ore and fossils.展开更多
基金supported by China Ministry of science and Technology(2000DEB20081)China Ocean Mineral Resources R&D Association(COMRA)(DY105-05-01-05)+1 种基金China Ministry of Education(205089)China National Natural Science Foundation(40076015).
文摘Marine sediments were dissolved by HNO3-HF-HC104 in a sealed container at low pressure; HF was evaporated in an open container and salts were dissolved in HCl by heating, then transferred to 2% HNO3 solution. A total of 45 elements, including Li, Be, Sc, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Cd, In, Sb, Cs, Ba, La, Ce, Pr, Nd, Sin, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Tl, Pb, Bi, Th and U, were measured by inductively coupled plasma mass spectrometry （ICP-MS）. Conditions and sample experiments showed that this procedure defines a good experimental method which has the advantages of clear interference, easy operation and reliable results. The concentrations of the 45 elements could be used for resource exploration, environmental assessment and academic research.
文摘Raohe honey (Honey in Raohe) is the only product which has obtained China’s national geographical mark for honey;however, it is always counterfeited by some producers due to its excellent quality. In this research, Raohe honey was identified by geographical sourcing, where the detection on 166 Raohe honey samples and 31 non-Raohe honey samples was conducted with Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Additionally, the method of Primary Composite Analysis accomplished dimensionality reduction by transforming the abundance ratios variables of 13 isotopes to 4 primary composites, and could explain 91.17% of the total variables. There were five models: Decision Tree, Naive Bayes, Neural Network, Partial Least Square Discriminate and Support Vector Machine, built on the four new variables of primary composites with the Agilent MPP Software. The validation of the models was performed with 11 Raohe honey samples and 5 non-Raohe honey samples randomly selected. The accuracies of the Decision Tree and Support Vector Machine models were both 93.97%, and those of the Naive Bayes and Neural Network models were both 87.5%, while the contribution rate of the Partial Least Square Discriminate model was only 75%. It was concluded that the Decision Tree and Support Vector Machine models could be used for indentifying Raohe honey, and the Naive Bayes and Neural Network models could work as references, while the Partial Least Square Discriminate model was not suitable for identifying Raohe honey.
文摘Individual monitoring of workers exposed to the risk of intake of actinides requires suitable methods for measuring low level of excreted activity. The current protocols used for actinides analysis in bioassay are usually complicated and highly time consuming. In this work, a protocol based on the microwave digestion of urines followed by the separation of actinides using calix[6]arene-based chromatography columns and their measurement by a quadrupole ICP-MS is developed and validated, for the first time, on urine samples containing the three actinides, U, Pu and Am. With this protocol, the total analysis time is about 2 days, including the mineralization of urine and the chromatographic separation of actinides. Detection limits of actinides in urine are determined and compared to those obtained after “dilute and shoot” ICP-MS analysis or after alpha spectrometry measurement.
基金Supported by Risk Monitoring Task Project of Chongqing Drug Administration in 2020。
文摘[Objectives]To detect content of Pb,Cd,Hg,As,Cu,Zn,and Cr in Lysimachia christinae,and to analyze the pollution level.[Methods]Seven kinds of elements in L.christinae were determined by Inductively coupled plasma mass spectrometry and analyzed by single index and comprehensive index.[Results]The seven heavy metal elements showed good linearity in their respective concentration ranges.The recoveries of the samples were 84.5%-109.5%,and the RSD values were 2.30%-5.10%.Comparing the measured results of heavy metal elements with the limit values stipulated in the 2020 edition of the Chinese Pharmacopoeia and other standards,the Cr element in 19 batches of samples exceeded the standard,and the Zn element in 7 batches of samples exceeded the standard.The exceeding rates were 100.0%and 36.8%,respectively;the content of other heavy metal elements did not exceed the standard.The order of individual index from large to small was Cr,Zn,Cd,Hg,Cu,As,and Pb,and the average comprehensive pollution level was mild pollution and above.[Conclusions]L.christinae was mainly polluted by Cr,followed by Zn;this study can provide basic data for drafting of the limit standard for heavy metal elements in L.christinae.
文摘A quick and sensitive method was developed for the determination of 19 metal elements in Saffron,a traditional Chinese medicinal herb,collected from Tibet Autonomous Region and Henan Province of China using inductively coupled plasma atomic emission spectrometry（ICP-AES）or inductively coupled plasma mass spectrometry（ICP-MS）.The determined 19 metals in Saffron include Ca,Fe,Mg,P,Sr,Al,Mn,Zn,V,Cr,Se,Co,Ni,Mo,and heavy metals As,Cu,Cd,Hg and Pb.For all the analyzed elements,the correlative coefficients of the calibration curves were no less than 0.9938.This proposed method was accurate,and the relative standard deviations of the measurements were lower than 5.25%.It can be used for the quality control of metal elements in Saffron.
文摘Thiols play vital roles in cellular metabolism knowledge of which may be important in the design of future anticancer drugs. Previous work on the composition of the thiols present in human cancer cell lines has shown the presence of an unknown low molecular weight species, deemed to be a “Conthiol”, which could be important in this respect. This was prepared and isolated from a human prostate cancer cell line (LNCaP) in the form of an adduct of 2-mercuri-4-nitrophenol;it accounts for 56.5% of the total cellular thiols present in this cell line. Initial LC-MS analysis of this adduct had indicated that the possible molecular weight of the thiol was in the region of 467 daltons. In further analytical studies to identify the thiol, attempts were made to release it from the adduct by passage through a Thiopropyl Sepharose6B column. LC-MS analysis of the column eluate revealed two components yielding negative ion fragments of 427 m/z and 449 m/z. Only the former component contained thiol, indicating that a breakdown and/or possible rearrangement of the Conthiol had occurred. Further investigations of the column thiol eluate using ICP-MS analysis showed that the sulfur content agreed with the spectrophotometric analysis result (Ellman assay) and that the molecule did not contain phosphate. Amino acid analyses of the eluate were negative. In an attempt to prevent the breakdown of the thiol released by the Thiopropyl Sepharose 6B column, the adduct was treated with 5% v/v bromine water prior to applying to the column. In this instance the thiol containing eluate obtained from the column was treated with an equimolar quantity of mercuric chloride forming a fresh adduct, RS-Hg-SR. LC-MS analysis of this mercurial adduct detected a negative ion fragment of 782 m/z which on further ionization gave a ladder like pattern showing loss of mass units of 58 in each rung. This would seem to suggest the presence of a repeat polymer like structure containing 5 monomers, which, plus the thiol atom, gives a possible formula weight of 322;probably revealing only a part of the unknown Conthiol molecule whose properties and formula weight do not correlate with any known cellular thiol. Further analysis of the thiol released from the adduct on the Thiopropyl Sepharose 6B column by Infra-red (FTIR) provided little information except to confirm the presence of the thiol group and C=O stretch bands together with the possibility of a lactam ring at 1651 and 1634 cm·s<sup>-</sup><sup>1</sup>.
基金supported by the National Natural Science Foundation of China(21727812,21705016,21864001)the Program for Changjiang Scholars and Innovative Research Team in University(PCSIRT)(IRT_17R20)Department of Science and Technology of Jiangxi Province(20192AEI91006)。
文摘At the beginning of rare earth industry,several days are normally required for characterization of rare earth elements(REEs)fractionation in ore samples.Herein,rapid fractionation analysis of 15 REEs and accompanied metal(Fe,Mn,etc.)in ore samples has been achieved within 1 h using ICP-MS with a homemade device for online sequential solvent extraction.As a result,five fractionations for REEs occurrences,i.e.,water soluble,exchangeable,reducible,oxidizable and crystalline,have been identified,offering chemical insights which not only reveal the formation mechanism of REEs ores but also show great implications for guiding the exploitation and separation of REEs.In comparison with conventional methods,the present approach significantly shortened the analysis time(1 h vs.~80 h)and reduced the sample consumption(1.0 mg vs.5.0 g)with high recovery(>95%),providing a useful platform for the rapid quantitative fractionation analysis of REEs in complexed samples such as ore and fossils.
