The quantitative determination of heavy metals in aquatic products is of great importance for food security issues.Laser-induced breakdown spectroscopy(LIBS)has been used in a variety of foodstuff analysis,but is stil...The quantitative determination of heavy metals in aquatic products is of great importance for food security issues.Laser-induced breakdown spectroscopy(LIBS)has been used in a variety of foodstuff analysis,but is still limited by its low sensitivity when targeting trace heavy metals.In this work,we compare three sample enrichment methods,namely drying,carbonization,and ashing,for increasing detection sensitivity by LIBS analysis for Pb and Cr in oyster samples.The results demonstrate that carbonization can remove a significant amount of the contributions of organic elements C,H,N and O;meanwhile,the signals of the metallic elements such as Cu,Pb,Sr,Ca,Cr and Mg are enhanced by3–6 times after carbonization,and further enhanced by 5–9 times after ashing.Such enhancement is not only due to the more concentrated metallic elements in the sample compared to the dried ones,but also the unifying of the matter in carbonized and ashed samples from which higher plasma temperature and electron density are observed.This condition favors the detection of trace elements.According to the calibration curves with univariate and multivariate analysis,the ashing method is considered to be the best choice.The limits of detection of the ashing method are 0.52 mg kg-1 for Pb and0.08 mg kg-1 for Cr,which can detect the presence of heavy metals in the oysters exceeding the maximum limits of Pb and Cr required by the Chinese national standard.This method provides a promising application for the heavy metal contamination monitoring in the aquatic product industry.展开更多
A sample enrichment method focusing on the minor targeted components was established to help them to be successfully separated by pH-zone refining CCC.Seven minor indole alkaloids in Uncaria rhynchophylla(Miq.)Miq.ex ...A sample enrichment method focusing on the minor targeted components was established to help them to be successfully separated by pH-zone refining CCC.Seven minor indole alkaloids in Uncaria rhynchophylla(Miq.)Miq.ex Havil(UR)were chosen to show the advantage of this method.The sample enrichment and separation were展开更多
A simple and rapid dispersive liquid-liquid microextraction(DLLME)technique coupled with gas chromatography-ion trap mass spectrometry(GC-MS)was developed for the extraction and analysis of five endosulfan pesticides ...A simple and rapid dispersive liquid-liquid microextraction(DLLME)technique coupled with gas chromatography-ion trap mass spectrometry(GC-MS)was developed for the extraction and analysis of five endosulfan pesticides from the fish pond water.In this work,different parameters affecting the extraction process such as the type and volume of extraction solvent,type and volume of disperser solvent,and extraction time were studied and optimized.Under optimized conditions,the enrichment factor ranged from 189 to 269 and the relative recovery ranged from 88.5%to 94.9%.The linear range was 2.0-80.0 mg/L;the limits of detection and quantitation were in the range 0.04-1.06 mg/L and 0.12-3.53 mg/L,respectively.The relative standard deviations were in the range 0.94%-2.08%(n D 5).The obtained results show that DLLME combined with GC-MS is a fast and simple method for the determination of endosulfan pesticides in fish pond water.展开更多
基金supported by the National Key Research and Development Program of China(No.2019YFD0901701)National Natural Science Foundation of China(Nos.12174359and 61975190)Provincial Key Research and Development Program of Shandong,China(No.2019GHZ010)。
文摘The quantitative determination of heavy metals in aquatic products is of great importance for food security issues.Laser-induced breakdown spectroscopy(LIBS)has been used in a variety of foodstuff analysis,but is still limited by its low sensitivity when targeting trace heavy metals.In this work,we compare three sample enrichment methods,namely drying,carbonization,and ashing,for increasing detection sensitivity by LIBS analysis for Pb and Cr in oyster samples.The results demonstrate that carbonization can remove a significant amount of the contributions of organic elements C,H,N and O;meanwhile,the signals of the metallic elements such as Cu,Pb,Sr,Ca,Cr and Mg are enhanced by3–6 times after carbonization,and further enhanced by 5–9 times after ashing.Such enhancement is not only due to the more concentrated metallic elements in the sample compared to the dried ones,but also the unifying of the matter in carbonized and ashed samples from which higher plasma temperature and electron density are observed.This condition favors the detection of trace elements.According to the calibration curves with univariate and multivariate analysis,the ashing method is considered to be the best choice.The limits of detection of the ashing method are 0.52 mg kg-1 for Pb and0.08 mg kg-1 for Cr,which can detect the presence of heavy metals in the oysters exceeding the maximum limits of Pb and Cr required by the Chinese national standard.This method provides a promising application for the heavy metal contamination monitoring in the aquatic product industry.
基金supported by the National Science and Technology Major Project for Major Drug Development(No.2013ZX09508104)the Traditional Chinese Medicine Industry Research Special Project(No.201307002)the National Science&Technology Major Project Key New Drug Creation and Manufacturing program(No.2011ZX09307002-03)of the People's Republic of China
文摘A sample enrichment method focusing on the minor targeted components was established to help them to be successfully separated by pH-zone refining CCC.Seven minor indole alkaloids in Uncaria rhynchophylla(Miq.)Miq.ex Havil(UR)were chosen to show the advantage of this method.The sample enrichment and separation were
文摘A simple and rapid dispersive liquid-liquid microextraction(DLLME)technique coupled with gas chromatography-ion trap mass spectrometry(GC-MS)was developed for the extraction and analysis of five endosulfan pesticides from the fish pond water.In this work,different parameters affecting the extraction process such as the type and volume of extraction solvent,type and volume of disperser solvent,and extraction time were studied and optimized.Under optimized conditions,the enrichment factor ranged from 189 to 269 and the relative recovery ranged from 88.5%to 94.9%.The linear range was 2.0-80.0 mg/L;the limits of detection and quantitation were in the range 0.04-1.06 mg/L and 0.12-3.53 mg/L,respectively.The relative standard deviations were in the range 0.94%-2.08%(n D 5).The obtained results show that DLLME combined with GC-MS is a fast and simple method for the determination of endosulfan pesticides in fish pond water.