Background:Cyperi Rhizoma,derived from Cyperus rotundus L.,is a widely used medicinal herb in traditional Chinese medicine(TCM),with Shandong Province recognized as its geo-authentic habitat.However,the quality of Cyp...Background:Cyperi Rhizoma,derived from Cyperus rotundus L.,is a widely used medicinal herb in traditional Chinese medicine(TCM),with Shandong Province recognized as its geo-authentic habitat.However,the quality of Cyperi Rhizoma varies significantly across different regions,potentially influencing its therapeutic efficacy.This study investigates the influence of geographic origin on the chemical composition and overall quality of Cyperi Rhizoma.Methods:A comprehensive approach,including traditional quality assessment,GC-MS(g as c hromatography-m ass s pectrometry),RP-HPLC(r everse p hase h igh-p erformance l iquid c hromatography),and FT-IR(f ourier t ransform i nfrared s pectroscopy)techniques,was employed to analyze Cyperi Rhizoma samples from Shandong Province.These methods examined the physical appearance,chemical profile,and content variations,particularly focusing onα-cyperone.Results:Traditional quality assessments revealed noticeable differences in the external characteristics of the samples.GC-MS analysis identified a variety of unique chemical constituents,while RP-HPLC and FT-IR showed significant variations inα-cyperone content,with higher levels found in Shandong samples.Conclusion:These results demonstrate that geographic origin is a critical determinant of Cyperi Rhizoma quality,with Shandong specimens exhibiting superiorα-cyperone levels and characteristic phytochemical profiles.This validates the geo-authenticity concept in TCM and provides actionable data for developing evidence-based quality standards,suggesting that provenance should be prioritized in medicinal material selection and pharmacopeial specifications.展开更多
To simultaneously enrich,separate,and determine five fluoroquinolone antibiotics(FQs)in marine crude drugs(MCDs),seawater and seafood,we conducted this study using vortex assisted dispersed liquid-liquid microextracti...To simultaneously enrich,separate,and determine five fluoroquinolone antibiotics(FQs)in marine crude drugs(MCDs),seawater and seafood,we conducted this study using vortex assisted dispersed liquid-liquid microextraction(DLLME),followed by capillary electrophoresis(CE)-UV.A single-variable optimization was employed to examine the factors influencing the separation effect of CE and the extraction efficiency of DLLME,including buffer solution,organic solvent,separation voltage,extractant,dispersant,and sample solution pH.Under the optimal conditions,the baseline separation of the five FQs was achieved within 6 min.The analytical performance of the method was assessed using six types of actual samples,including three MCDs of hippocampus,clam,and kelp,seawater,and two seafood of prawn and pomfret,demonstrating good linearity ranging from 0.1-5 or 0.01-5μg/mL.The limits of detection(LODs)and limits of quantification(LOQs)for the five FQs in MCDs were 0.0022-0.0292 and 0.0066-0.0973μg/mL,respectively.The LODs and LOQs in seawater and seafood were 0.0009-0.0262 and 0.0029-0.0874μg/mL,respectively.The matrix effects of this method were evaluated in the hippocampus,seawater,and prawn,and the results show that DLLME could effectively eliminate matrix interference.Satisfactory recovery rates were achieved in all the six tested actual samples.This developed DLLME-CE method was proven simple to operate,accurate and reliable,with high sensitivity,making it suitable for the analysis of multiple antibiotic residues in complex matrices.展开更多
A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 pol...A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 polycyclic aromatic hydrocarbons(PAHs),70 polychlorinated biphenyls(PCBs),123 pesticides,20 phthalate esters(PAEs),4 organophosphate esters(OPEs),9 synthetic musks(SMs),and 5 UV filters(UVs)in water.No-tably,this method provided a decent linearity of calibration standards(R^(2)>0.999),excellent method limits of quantification(MLOQs)(0.12–11.41 ng/L),satisfactory matrix spiking recovery rates(60.4%–126%),and high precision(intra-day relative standard deviations(RSDs):1.0%–10.0%,inter-day RSDs:3.0%–15.0%,and inter-week RSDs:3.4%–15.7%),making it suitable for trace-level studies.Statistical analysis revealed that SVOCs with higher volatility exhibited enhanced recovery rates.Validation of the methodology involved analyzing SVOCs in real spring water and river water samples.Twenty-seven SVOCs were detected in spring water and 58 in river water,with an average concentration of 631.73 and 16,095 ng/L,respectively.Among the detected SVOCs,PAEs constituted the predominant proportion.This study underscored the presence of SVOCs contamination specifi-cally within the spring water,although SVOCs concentrations in river water were significantly greater than those found in spring water.In summary,this sensitive method based on SPE–GC–MS/MS was successfully developed and validated for the rapid analysis of a diverse array of 256 SVOCs at trace levels in water,including not only the traditional highly valued PAHs,PCBs,pesticides,and PAEs,but also the emerging OPEs,UVs,and SMs.展开更多
基金supported by the National Natural Science Foundation of China(No.82204610)Qihang Talent Program(L2022046)+1 种基金the Scientific and Technological Innovation Project of China Academy of Chinese Medical Sciences(CI2021A04013)Fundamental Research Funds for the Central Public Welfare Research Institutes(ZZ15-YQ-041 and L2021029).
文摘Background:Cyperi Rhizoma,derived from Cyperus rotundus L.,is a widely used medicinal herb in traditional Chinese medicine(TCM),with Shandong Province recognized as its geo-authentic habitat.However,the quality of Cyperi Rhizoma varies significantly across different regions,potentially influencing its therapeutic efficacy.This study investigates the influence of geographic origin on the chemical composition and overall quality of Cyperi Rhizoma.Methods:A comprehensive approach,including traditional quality assessment,GC-MS(g as c hromatography-m ass s pectrometry),RP-HPLC(r everse p hase h igh-p erformance l iquid c hromatography),and FT-IR(f ourier t ransform i nfrared s pectroscopy)techniques,was employed to analyze Cyperi Rhizoma samples from Shandong Province.These methods examined the physical appearance,chemical profile,and content variations,particularly focusing onα-cyperone.Results:Traditional quality assessments revealed noticeable differences in the external characteristics of the samples.GC-MS analysis identified a variety of unique chemical constituents,while RP-HPLC and FT-IR showed significant variations inα-cyperone content,with higher levels found in Shandong samples.Conclusion:These results demonstrate that geographic origin is a critical determinant of Cyperi Rhizoma quality,with Shandong specimens exhibiting superiorα-cyperone levels and characteristic phytochemical profiles.This validates the geo-authenticity concept in TCM and provides actionable data for developing evidence-based quality standards,suggesting that provenance should be prioritized in medicinal material selection and pharmacopeial specifications.
基金Supported by the National Natural Science Foundation of China(No.22176210)the Major Innovation Fund of Shandong Province(No.2021ZDSYS23)。
文摘To simultaneously enrich,separate,and determine five fluoroquinolone antibiotics(FQs)in marine crude drugs(MCDs),seawater and seafood,we conducted this study using vortex assisted dispersed liquid-liquid microextraction(DLLME),followed by capillary electrophoresis(CE)-UV.A single-variable optimization was employed to examine the factors influencing the separation effect of CE and the extraction efficiency of DLLME,including buffer solution,organic solvent,separation voltage,extractant,dispersant,and sample solution pH.Under the optimal conditions,the baseline separation of the five FQs was achieved within 6 min.The analytical performance of the method was assessed using six types of actual samples,including three MCDs of hippocampus,clam,and kelp,seawater,and two seafood of prawn and pomfret,demonstrating good linearity ranging from 0.1-5 or 0.01-5μg/mL.The limits of detection(LODs)and limits of quantification(LOQs)for the five FQs in MCDs were 0.0022-0.0292 and 0.0066-0.0973μg/mL,respectively.The LODs and LOQs in seawater and seafood were 0.0009-0.0262 and 0.0029-0.0874μg/mL,respectively.The matrix effects of this method were evaluated in the hippocampus,seawater,and prawn,and the results show that DLLME could effectively eliminate matrix interference.Satisfactory recovery rates were achieved in all the six tested actual samples.This developed DLLME-CE method was proven simple to operate,accurate and reliable,with high sensitivity,making it suitable for the analysis of multiple antibiotic residues in complex matrices.
基金supported by the National Natural Science Foundation of China(No.51939009)Shenzhen Science and Technology Program(Nos.JCYJ20241202125905008 and GXWD20201231165807007-20200810165349001).
文摘A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 polycyclic aromatic hydrocarbons(PAHs),70 polychlorinated biphenyls(PCBs),123 pesticides,20 phthalate esters(PAEs),4 organophosphate esters(OPEs),9 synthetic musks(SMs),and 5 UV filters(UVs)in water.No-tably,this method provided a decent linearity of calibration standards(R^(2)>0.999),excellent method limits of quantification(MLOQs)(0.12–11.41 ng/L),satisfactory matrix spiking recovery rates(60.4%–126%),and high precision(intra-day relative standard deviations(RSDs):1.0%–10.0%,inter-day RSDs:3.0%–15.0%,and inter-week RSDs:3.4%–15.7%),making it suitable for trace-level studies.Statistical analysis revealed that SVOCs with higher volatility exhibited enhanced recovery rates.Validation of the methodology involved analyzing SVOCs in real spring water and river water samples.Twenty-seven SVOCs were detected in spring water and 58 in river water,with an average concentration of 631.73 and 16,095 ng/L,respectively.Among the detected SVOCs,PAEs constituted the predominant proportion.This study underscored the presence of SVOCs contamination specifi-cally within the spring water,although SVOCs concentrations in river water were significantly greater than those found in spring water.In summary,this sensitive method based on SPE–GC–MS/MS was successfully developed and validated for the rapid analysis of a diverse array of 256 SVOCs at trace levels in water,including not only the traditional highly valued PAHs,PCBs,pesticides,and PAEs,but also the emerging OPEs,UVs,and SMs.
