[Objectives]To investigate the content and distribution of inorganic elements in Astragalus membranaceus sourced from various regions in Gansu Province.[Methods]28 batches of A.membranaceus samples were collected and ...[Objectives]To investigate the content and distribution of inorganic elements in Astragalus membranaceus sourced from various regions in Gansu Province.[Methods]28 batches of A.membranaceus samples were collected and subsequently digested using the Multiwave 7000 super microwave digestion system.The contents of aluminum(Al),barium(Ba),beryllium(Be),cobalt(Co),chromium(Cr),iron(Fe),gallium(Ga),magnesium(Mg),manganese(Mn),nickel(Ni),antimony(Sb),tin(Sn),strontium(Sr),titanium(Ti),thallium(Tl),vanadium(V),and zinc(Zn)were quantified utilizing a PerkinElmer 2000 inductively coupled plasma mass spectrometer.Principal component analysis was performed utilizing SPSS 25.0 to identify the distinctive characteristic elements of A.membranaceus.Additionally,systematic cluster analysis was conducted using these characteristic elements as variables to investigate the relationship between the primary inorganic elements and the geographical origin of A.membranaceus.[Results]17 inorganic elements were identified in A.membranaceus specimens collected from Gansu Province,with characteristic elements including Ba,Co,Fe,Ga,Mn,Zn,and Sn.The contents of inorganic elements in various sources of A.membranaceus exhibited significant variability and demonstrated distinct clustering characteristics.[Conclusions]A.membranaceus,originating from Gansu Province,exhibits a high content of inorganic elements.However,variations in ecological environments can lead to differences in the specific inorganic elements that are enriched.This study aims to provide a reference for the further development and application of A.membranaceus.展开更多
Operating an Agilent 7700X ICP-MS spectrometer under robust plasma conditions (1550 W) with a He-filled octopole collision cell and analysing solutions (?1 total dissolved solids) still suffered analyte peak suppressi...Operating an Agilent 7700X ICP-MS spectrometer under robust plasma conditions (1550 W) with a He-filled octopole collision cell and analysing solutions (?1 total dissolved solids) still suffered analyte peak suppression due to matrix effects. International reference rocks BCR-1, BHVO-1, AGV-1, G-2 and BCR-2 all showed count rate reductions for 36 elements (mass range 7Li to 238U) averaging ~10% but with no dependence on isotope mass. Use of an internal standard (103Rh) and/or using a ten-fold dilution of sample solutions reduced these effects but problems with reduced count rates combined with larger errors for some elements introduced other problems. The best approach was to normalise the count rates for each element in the other samples against those for BCR-1 as an external standard;thus the count suppression due to the matrix effect is corrected for each individual element. This approach provides standardization “traceability” in line with the ERM ISO/IEC requirement. Experiments are also reported on quantifying the proportions of Ba and selected REE oxide/hydroxide components versus parent isotopes (XO/X and XOH/X). This information is essential for correcting peak interferences on higher mass number REE for the rock samples, and equations are developed to use measured CeO/Ce and CeOH/Ce ratios to predict such values for any other member of the REE suite. Concentrations obtained show excellent agreement with recommended values for the international reference materials especially for the REE. Robust data are also provided for two other standard rocks: nepheline syenite STM-1 and quartz syenite CAAS-1;the latter shows exceptional enrichments of Zr, REE, Th, and U.展开更多
目的 建立电感耦合等离子体质谱法(inductively coupled plasma-mass spectrometry,ICP-MS)测定注射用亚锡甲氧异腈中元素杂质的含量。方法 样品溶解后,采用ICP-MS半定量测定模式对注射用亚锡甲氧异腈中元素杂质进行初步筛查,结合国际...目的 建立电感耦合等离子体质谱法(inductively coupled plasma-mass spectrometry,ICP-MS)测定注射用亚锡甲氧异腈中元素杂质的含量。方法 样品溶解后,采用ICP-MS半定量测定模式对注射用亚锡甲氧异腈中元素杂质进行初步筛查,结合国际人用药品注册技术协调会(International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use,ICH)Q3D元素杂质指导原则的要求,确定16种元素:锂(Li)、镁(Mg)、铝(Al)、硅(Si)、钾(K)、钒(V)、铁(Fe)、钴(Co)、镍(Ni)、锌(Zn)、砷(As)、镉(Cd)、铟(In)、锑(Sb)、汞(Hg)和铅(Pb)作为定量考察和控制的元素杂质研究对象。ICP-MS采集模式选择动能歧视模式进行定量方法研究,分别以钪(Sc)、锗(Ge)、钇(Y)、铋(Bi)作为内标,测定16种元素杂质的含量。结果 16种元素杂质在各自线性范围内响应与浓度相关性良好(r≥0.999 3);方法精密度(RSD≤3.53%)和重复性(RSD≤3.69%)均较好;各元素平均回收率为95.86%~105.64%(RSD≤5.06%,n=9),方法准确性良好。注射用亚锡甲氧异腈样品中16种元素均未超出限度,Mg、K、Zn 3种元素含量相对较高。结论 金属盐类制剂产品可能引入ICH Q3D原则要求以外的元素杂质。本研究建立的ICP-MS定量方法简便、快速,可用于注射用亚锡甲氧异腈中元素杂质的筛查、检测和风险评估。展开更多
基金Supported by Project of NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine(2023GSMPA-KL06,2024GSMPA-KL16).
文摘[Objectives]To investigate the content and distribution of inorganic elements in Astragalus membranaceus sourced from various regions in Gansu Province.[Methods]28 batches of A.membranaceus samples were collected and subsequently digested using the Multiwave 7000 super microwave digestion system.The contents of aluminum(Al),barium(Ba),beryllium(Be),cobalt(Co),chromium(Cr),iron(Fe),gallium(Ga),magnesium(Mg),manganese(Mn),nickel(Ni),antimony(Sb),tin(Sn),strontium(Sr),titanium(Ti),thallium(Tl),vanadium(V),and zinc(Zn)were quantified utilizing a PerkinElmer 2000 inductively coupled plasma mass spectrometer.Principal component analysis was performed utilizing SPSS 25.0 to identify the distinctive characteristic elements of A.membranaceus.Additionally,systematic cluster analysis was conducted using these characteristic elements as variables to investigate the relationship between the primary inorganic elements and the geographical origin of A.membranaceus.[Results]17 inorganic elements were identified in A.membranaceus specimens collected from Gansu Province,with characteristic elements including Ba,Co,Fe,Ga,Mn,Zn,and Sn.The contents of inorganic elements in various sources of A.membranaceus exhibited significant variability and demonstrated distinct clustering characteristics.[Conclusions]A.membranaceus,originating from Gansu Province,exhibits a high content of inorganic elements.However,variations in ecological environments can lead to differences in the specific inorganic elements that are enriched.This study aims to provide a reference for the further development and application of A.membranaceus.
文摘Operating an Agilent 7700X ICP-MS spectrometer under robust plasma conditions (1550 W) with a He-filled octopole collision cell and analysing solutions (?1 total dissolved solids) still suffered analyte peak suppression due to matrix effects. International reference rocks BCR-1, BHVO-1, AGV-1, G-2 and BCR-2 all showed count rate reductions for 36 elements (mass range 7Li to 238U) averaging ~10% but with no dependence on isotope mass. Use of an internal standard (103Rh) and/or using a ten-fold dilution of sample solutions reduced these effects but problems with reduced count rates combined with larger errors for some elements introduced other problems. The best approach was to normalise the count rates for each element in the other samples against those for BCR-1 as an external standard;thus the count suppression due to the matrix effect is corrected for each individual element. This approach provides standardization “traceability” in line with the ERM ISO/IEC requirement. Experiments are also reported on quantifying the proportions of Ba and selected REE oxide/hydroxide components versus parent isotopes (XO/X and XOH/X). This information is essential for correcting peak interferences on higher mass number REE for the rock samples, and equations are developed to use measured CeO/Ce and CeOH/Ce ratios to predict such values for any other member of the REE suite. Concentrations obtained show excellent agreement with recommended values for the international reference materials especially for the REE. Robust data are also provided for two other standard rocks: nepheline syenite STM-1 and quartz syenite CAAS-1;the latter shows exceptional enrichments of Zr, REE, Th, and U.
文摘目的 建立电感耦合等离子体质谱法(inductively coupled plasma-mass spectrometry,ICP-MS)测定注射用亚锡甲氧异腈中元素杂质的含量。方法 样品溶解后,采用ICP-MS半定量测定模式对注射用亚锡甲氧异腈中元素杂质进行初步筛查,结合国际人用药品注册技术协调会(International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use,ICH)Q3D元素杂质指导原则的要求,确定16种元素:锂(Li)、镁(Mg)、铝(Al)、硅(Si)、钾(K)、钒(V)、铁(Fe)、钴(Co)、镍(Ni)、锌(Zn)、砷(As)、镉(Cd)、铟(In)、锑(Sb)、汞(Hg)和铅(Pb)作为定量考察和控制的元素杂质研究对象。ICP-MS采集模式选择动能歧视模式进行定量方法研究,分别以钪(Sc)、锗(Ge)、钇(Y)、铋(Bi)作为内标,测定16种元素杂质的含量。结果 16种元素杂质在各自线性范围内响应与浓度相关性良好(r≥0.999 3);方法精密度(RSD≤3.53%)和重复性(RSD≤3.69%)均较好;各元素平均回收率为95.86%~105.64%(RSD≤5.06%,n=9),方法准确性良好。注射用亚锡甲氧异腈样品中16种元素均未超出限度,Mg、K、Zn 3种元素含量相对较高。结论 金属盐类制剂产品可能引入ICH Q3D原则要求以外的元素杂质。本研究建立的ICP-MS定量方法简便、快速,可用于注射用亚锡甲氧异腈中元素杂质的筛查、检测和风险评估。
