Plasma quinolone concentrations are not routinely measured in clinical practice.However,in order to optimize quinolone treatment,monitoring of plasma concentrations could sometimes be useful particularly in critically...Plasma quinolone concentrations are not routinely measured in clinical practice.However,in order to optimize quinolone treatment,monitoring of plasma concentrations could sometimes be useful particularly in critically ill patients.In this study,anti-sparfloxacin antibody was obtained by immunizing rabbits with sparfloxacin conjugated with bovine serum albumin using isobutyl chloroformate method.After the assay procedure was optimized,the standard curve of sparfloxacin was established.The practical measuring range of the competitive ELISA extended from 5 ng/mL to 2 mg/mL.The recovery rates and coefficients of variation for rat plasma,urine and tissues were 87.7-106.2% and 4.8-15.3%,respectively.To demonstrate the potential of the ELISA,a preliminary pharmacokinetics and tissue distribution study of sparfloxacin in rats and quantitative analysis of sparfloxacin in several pharmaceuticals were performed and compared with high-performance liquid chromatography(HPLC).The experimental data indicated that the proposed method would be a valuable tool in therapeutic drug monitoring(TDM) for sparfloxacin.展开更多
In this study,a functionalized covalent-organic framework(COF)was first synthesized using porphyrin as the fabrication unit and showed an edge-curled,petal-like and well-ordered structure.The synthesized COF was then ...In this study,a functionalized covalent-organic framework(COF)was first synthesized using porphyrin as the fabrication unit and showed an edge-curled,petal-like and well-ordered structure.The synthesized COF was then introduced to prepare porous organic polymer monolithic materials(POPMs).Two composite POPM/COF monolithic materials with rod shapes,referred to as sorbent A and sorbent B,were prepared in stainless steel tubes using different monomers.Sorbents A and B exhibited relatively uniform porous structures and enhanced specific surface areas of 153.14 m;/g and 80.01 m;/g,respectively.The prepared composite monoliths were used as in-tube solid-phase extraction(SPE)sorbents combined with HPLC for the on-line extraction and quantitative analytical systems.Indole alkaloids(from Catharanthus roseus G.Don and Uncaria rhynchophylla(Miq.)Miq.Ex Havil.)contained in mouse plasma were extracted and quantitatively analyzed using the online system.The two composite multifunctional monoliths showed excellent clean-up ability for complex biological matrices,as well as superior selectivity for target indole alkaloids.Method validation showed that the RSD values of the repeatability(n=6)were≤3.46%,and the accuracy expressed by the spiked recoveries was in the ranges of 99.38%-100.91%and 96.39%-103.50%for vinca alkaloids and Uncaria alkaloids,respectively.Furthermore,sorbents A and B exhibited strong reusability,with RSD values≤5.32%,which were based on the peak area of the corresponding alkaloids with more than 100 injections.These results indicate that the composite POPM/COF rod-shaped monoliths are promising media as SPE sorbents for extracting trace compounds in complex biological samples.展开更多
Type 1 Diabetes mellitus (T1DM) is one of the familiar childhood immune-mediated onsets and can lead to early mortalities and morbidities. It can arise at any stage, but the peak of occurrence is reported less than 18...Type 1 Diabetes mellitus (T1DM) is one of the familiar childhood immune-mediated onsets and can lead to early mortalities and morbidities. It can arise at any stage, but the peak of occurrence is reported less than 18 years of age. T1DM cases in Pakistan were less than 2% of the total diabetic population. The current work designed to assess the concentration of cadmium (Cd) and zinc (Zn) in blood, scalp hair and serum samples of T1DM children, age ranged 1 - 14 years of both genders. For comparison purpose, the age-matched referent subjects of both genders were tested. The microwave-assisted acid digestion procedure was used to determine the elemental analysis in the biological samples of T1DM children and referent subjects. The resulted data of certified reference material of blood, scalp hair, and serum validated the certainty of the designed method. The analysis of Zn was performed by flame atomic absorption spectrometry, while the Cd contents were determined by electrothermal atomic absorption spectrometry. T1DM affected children of both genders have lower Zn level in the blood, scalp hair, and serum samples. Whereas, the levels of Cd were found to be higher in the biological samples of T1DM affected children as compared to referent subjects. The finding of the current study is a significant hypothesis for medical experts, to diagnose the deficiency of essential (Zn) and toxicity of heavy/toxic element (Cd) in the biological specimen of T1DM affected children.展开更多
Workers of the Lakhra coal mining Sindh Pakistan were affected by a multi-factorial exposure of heavy metals. The prevalence of lead (Pb) exposures in work-related symptoms among workers of indoor and outdoor mining o...Workers of the Lakhra coal mining Sindh Pakistan were affected by a multi-factorial exposure of heavy metals. The prevalence of lead (Pb) exposures in work-related symptoms among workers of indoor and outdoor mining of Lakhra coal mining was evaluated in detail. The biological samples (scalp hair and blood) of 270 workers of Lakhra coal mining {official and control subjects} (indoor and outdoor) 18 to 55 years age group and 70 referent subjects of same age-groups were examined. The biological samples (blood and scalp hair) of workers of Lakhra coal mining and referent subjects were analyzed for calcium (Ca) and lead (Pb). Flame atomic absorption spectrometry was applied for the determination of the Ca in digested samples of studied subjects by the microwave oven whereas, the Pb contents were measured by electrothermal atomic absorption spectrometry. The validity of the methodology was checked by using the certified human hair material (BCR 397) and lyophilized human blood (Clincheck). The results indicated the higher contents of Pb in biological samples of indoor and outdoor mining workers than referents. However, the levels of Ca were found to be lower in indoor and outdoor mining workers than those of referents. It can be concluded that immediate action should be taken by recommended authorities to improve the ventilation and hygiene practices inside the industries, mines, and other workplaces.展开更多
<strong>Background:</strong> Recently, Coronavirus Disease 2019 (COVID-19) has been affected by the extreme acute respiratory syndrome coronavirus 2 (SARS-CoV-2) and has developed important global health a...<strong>Background:</strong> Recently, Coronavirus Disease 2019 (COVID-19) has been affected by the extreme acute respiratory syndrome coronavirus 2 (SARS-CoV-2) and has developed important global health anxiety. At this time, the treatment options for this disease are only moderately successful. Smoking has been related to COVID-19 and its mortality, and it has the potential to affect bacteriological and viral conversion, clinical effects, and treatment outcomes. <strong>Methods:</strong> The aim of this study was to determine the relationship between critical essential trace {zinc (Zn), iron (Fe), and copper (Cu)} and toxic {cadmium (Cd) and nickel (Ni)} elements in human biological samples such as scalp hair, serum, saliva, blood, nasal fluid, and sputum of smoking and nonsmoking male COVID-19 patients (n = 139, age range 25 - 38 years) from Hyderabad, Pakistan. For comparative purposes, the biological specimens of referent persons (n = 83), pulmonary Tuberculosis (T.B) patients (n = 67), Pneumonia (n = 56) of the same age groups were also be analyzed. Microwave oven mediated digestion method was employed, and digestion of samples was carried out with the help of 2:1 mixture solution of HNO<sub>3</sub> (65%) and H<sub>2</sub>O<sub>2</sub> (30%). Atomic absorption spectrometry was employed for the determination of elemental concentrations from the microwave oven employed digested samples. <strong>Results:</strong> The found average of essential elements (Zn, Fe, and Cu) in biological specimens of smoker and nonsmoker male COVID-19, T.B, and Pneumonia patients was found to lower, whilst cadmium and nickel were found to be higher when compared with samples from referents (p < 0.001). <strong>Conclusions:</strong> Improved elemental (Cu, Fe, Zn) concentrations may also decrease the risk of bacterial co-infection by enhancing the mucociliary clearance and respiratory epithelial barrier function, in addition to providing direct antibacterial effects against <i>S. pneumoniae</i>. Our findings also suggest that higher Cd and Ni concentrations are linked to cigarette smoking, which could lead to COVID-19 and other lung-infected diseased recurrences. However, further clinical and experimental research is required.展开更多
Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sam...Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sample processing. To meet these emerging demands on biopharmaceutical analysis, this paper summarizes several new techniques of on-line biological sample processing: solid phase extraction, solid phase micro-extraction, column switching, limited intake filler, molecularly imprinted solid phase extraction,tubular column, and micro-dialysis. We describe new developments, principles, and characteristics of these techniques, and the application of liquid chromatography–mass spectrometry(LC–MS) in biopharmaceutical analysis with these new techniques in on-line biological sample processing.展开更多
Ascorbic acid(AA) serves as a key coenzyme in many metabolic pathways. Enough daily AA supplements from different dietary sources are the only way for human to maintain their AA levels in body.Determination of AA cont...Ascorbic acid(AA) serves as a key coenzyme in many metabolic pathways. Enough daily AA supplements from different dietary sources are the only way for human to maintain their AA levels in body.Determination of AA content in different foods guides to build healthy diet, which is of great biomedical significance. Hence, developing a highly selective and instantaneous fluorescent nanoprobe for the detection of AA in biological samples is highly needed. Here we present a novel turn-on fluorescent nanoprobe using lanthanide-doped upconversion nanoparticles(UCNPs) and cobalt oxyhydroxide(Co OOH) nanoflakes for monitoring AA in fruit samples. In this nanosystem, the UCNPs can be adsorbed onto the Co OOH nanoflakes, leading to a remarkable fluorescence decrease through Fo?rster resonance energy transfer. Furthermore, the AA could trigger the disassembly of the Co OOH to liberate the upconverted fluorescence. The UCNPs-based nanoprobe can provide an effective platform for highly selective and rapid detection of AA in biological samples.展开更多
In order to control drug crime effectively,it is necessary to develop selective analytical methods suitable for unambiguous identification and determination of drugs in illicit samples and biological matrices.A novel ...In order to control drug crime effectively,it is necessary to develop selective analytical methods suitable for unambiguous identification and determination of drugs in illicit samples and biological matrices.A novel microextraction technique based on ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction,(UA-LDS-DLLME)has been applied to the determination of four amphetamines(methamphetamine,amphetamine,3,4-methylenedioxymethamphetamine,and 3,4-methylenedioxyamphetamine)in urine samples by gas chromatography-mass spectrometry.The parameters affecting extraction efficiency have been investigated and optimized.UA-LDS-DLLME used ultrasound energy to assist in the emulsification process without any disperser solvent.Under the optimized conditions,linearity was observed for all analytes in the 0.15-10 p,g/mL range with correlation coefficients(R)ranging from 0.9886 to 0.9894.The recoveries of75.6-91.4%with relative standard deviations of 2.5-4.0%were obtained.The limits of detection(S/N=3)were estimated to be in the 5-10 ng/mL range.The UA-LDS-DLLME technique had the advantages of shorter extraction time,suitability for simultaneous pretreatments of batches of samples,and the higher extraction efficiency.It was successfully applied to the analysis of amphetamines in real human urine samples.展开更多
A rapid,accurate,and sensitive analytical method,ultrasonication-assisted spraying based fine droplet formationeliquid phase microextractionegas chromatographyemass spectrometry(UA-SFDF-LPME-GCMS),was proposed for the...A rapid,accurate,and sensitive analytical method,ultrasonication-assisted spraying based fine droplet formationeliquid phase microextractionegas chromatographyemass spectrometry(UA-SFDF-LPME-GCMS),was proposed for the determination of trace amounts of hydroxychloroquine sulfate in human serum,urine,and saliva samples.To determine the best extraction strategy,several liquid and solid phase extraction methods were investigated for their efficiencies in isolation and preconcentration of hydroxychloroquine sulfate from biological matrices.The UA-SFDF-LPME method was determined to be the best extraction method as it was operationally simple and provided accurate results.Variables such as the extraction solvent,spraying number,sodium hydroxide concentration and volume,sample volume,mixing method,and mixing period were optimized for the proposed method using the onevariable-at-a-time approach.In addition,Tukey’s method based on a post hoc comparison test was employed to evaluate the significant difference between the parameters inspected.After the optimization studies,the limit of detection(LOD)and limit of quantification(LOQ)were determined to be 0.7 and 2.4 mg/kg,respectively.The sensitivity of the GC-MS system based on the LOD was enhanced approximately 440-fold when the UA-SFDF-LPME method was employed.Spiking experiments were also conducted for the human serum,urine,and saliva samples to determine the applicability and accuracy of the proposed method.Recoveries for the human serum,urine,and saliva samples were found to be in the ranges of 93.9%-101.7%,95.2%-105.0%,and 93.1%-102.3%,respectively.These results were satisfactory and indicated that the hydroxychloroquine sulfate level in the above biological samples could be analyzed using the proposed method.展开更多
A method was established for the analysis of omethoate and it’s concomitants and decomposed product in biological samples by GC-MS.This method is rapid,reliable and accurate.
Objective:To assess the thorium exposure of the mine workers and the public to a typical rare earth mine and estimate the resultant committed effective dose to them.Methods:A total of 79 volunteers were selected in th...Objective:To assess the thorium exposure of the mine workers and the public to a typical rare earth mine and estimate the resultant committed effective dose to them.Methods:A total of 79 volunteers were selected in this survey,including 69 mine workers and 10 local residents living about 4 km away from the mine site.Urinary samples were collected from 79 volunteers,with 65 hair samples from 57 workers and 8 local residents.The thorium concentrations in urinary and hair samples were determined by using inductively coupled plasma mass spectrometry.The committed effective doses were estimated based on the urinary samples collected and the parameters as recommended by ICRP Publication 137.Results:Thorium concentrations in the samples from the workers ranged from 19.0 to 2388.8 ng/g in hair with median of 149.8 ng/g,and in urine 18.3–906.1 ng/L with median of 59.6 ng/L,respectively.The median values of thorium concentrations were 11.8 ng/g in hair and 32.40 ng/L in urine for the public respectively.The thorium concentrations in urinary and hair samples of the workers were not only higher than those of the residents in the local area,but also than those of non-occupationally exposed populations as reported.The median values of committed effective dose were estimated to be 1.51 mSv for the workers and 781μSv for the local residents,respectively.Conclusions:The residents in the local area,and especially the workers,have been subject to long term thorium exposure.More attention should be paid to the radiological hazards of thorium to the workers and local residents.展开更多
文摘Plasma quinolone concentrations are not routinely measured in clinical practice.However,in order to optimize quinolone treatment,monitoring of plasma concentrations could sometimes be useful particularly in critically ill patients.In this study,anti-sparfloxacin antibody was obtained by immunizing rabbits with sparfloxacin conjugated with bovine serum albumin using isobutyl chloroformate method.After the assay procedure was optimized,the standard curve of sparfloxacin was established.The practical measuring range of the competitive ELISA extended from 5 ng/mL to 2 mg/mL.The recovery rates and coefficients of variation for rat plasma,urine and tissues were 87.7-106.2% and 4.8-15.3%,respectively.To demonstrate the potential of the ELISA,a preliminary pharmacokinetics and tissue distribution study of sparfloxacin in rats and quantitative analysis of sparfloxacin in several pharmaceuticals were performed and compared with high-performance liquid chromatography(HPLC).The experimental data indicated that the proposed method would be a valuable tool in therapeutic drug monitoring(TDM) for sparfloxacin.
基金supported by the Natural Science Foundation of Hebei Province (Grant No.: B2020201002)the National Natural Science Foundation of China (Grant Nos.: 21974034 and 21505030)the Interdisciplinary Research Project of Natural Science of Hebei University (Grant No.: DXK201912)
文摘In this study,a functionalized covalent-organic framework(COF)was first synthesized using porphyrin as the fabrication unit and showed an edge-curled,petal-like and well-ordered structure.The synthesized COF was then introduced to prepare porous organic polymer monolithic materials(POPMs).Two composite POPM/COF monolithic materials with rod shapes,referred to as sorbent A and sorbent B,were prepared in stainless steel tubes using different monomers.Sorbents A and B exhibited relatively uniform porous structures and enhanced specific surface areas of 153.14 m;/g and 80.01 m;/g,respectively.The prepared composite monoliths were used as in-tube solid-phase extraction(SPE)sorbents combined with HPLC for the on-line extraction and quantitative analytical systems.Indole alkaloids(from Catharanthus roseus G.Don and Uncaria rhynchophylla(Miq.)Miq.Ex Havil.)contained in mouse plasma were extracted and quantitatively analyzed using the online system.The two composite multifunctional monoliths showed excellent clean-up ability for complex biological matrices,as well as superior selectivity for target indole alkaloids.Method validation showed that the RSD values of the repeatability(n=6)were≤3.46%,and the accuracy expressed by the spiked recoveries was in the ranges of 99.38%-100.91%and 96.39%-103.50%for vinca alkaloids and Uncaria alkaloids,respectively.Furthermore,sorbents A and B exhibited strong reusability,with RSD values≤5.32%,which were based on the peak area of the corresponding alkaloids with more than 100 injections.These results indicate that the composite POPM/COF rod-shaped monoliths are promising media as SPE sorbents for extracting trace compounds in complex biological samples.
文摘Type 1 Diabetes mellitus (T1DM) is one of the familiar childhood immune-mediated onsets and can lead to early mortalities and morbidities. It can arise at any stage, but the peak of occurrence is reported less than 18 years of age. T1DM cases in Pakistan were less than 2% of the total diabetic population. The current work designed to assess the concentration of cadmium (Cd) and zinc (Zn) in blood, scalp hair and serum samples of T1DM children, age ranged 1 - 14 years of both genders. For comparison purpose, the age-matched referent subjects of both genders were tested. The microwave-assisted acid digestion procedure was used to determine the elemental analysis in the biological samples of T1DM children and referent subjects. The resulted data of certified reference material of blood, scalp hair, and serum validated the certainty of the designed method. The analysis of Zn was performed by flame atomic absorption spectrometry, while the Cd contents were determined by electrothermal atomic absorption spectrometry. T1DM affected children of both genders have lower Zn level in the blood, scalp hair, and serum samples. Whereas, the levels of Cd were found to be higher in the biological samples of T1DM affected children as compared to referent subjects. The finding of the current study is a significant hypothesis for medical experts, to diagnose the deficiency of essential (Zn) and toxicity of heavy/toxic element (Cd) in the biological specimen of T1DM affected children.
文摘Workers of the Lakhra coal mining Sindh Pakistan were affected by a multi-factorial exposure of heavy metals. The prevalence of lead (Pb) exposures in work-related symptoms among workers of indoor and outdoor mining of Lakhra coal mining was evaluated in detail. The biological samples (scalp hair and blood) of 270 workers of Lakhra coal mining {official and control subjects} (indoor and outdoor) 18 to 55 years age group and 70 referent subjects of same age-groups were examined. The biological samples (blood and scalp hair) of workers of Lakhra coal mining and referent subjects were analyzed for calcium (Ca) and lead (Pb). Flame atomic absorption spectrometry was applied for the determination of the Ca in digested samples of studied subjects by the microwave oven whereas, the Pb contents were measured by electrothermal atomic absorption spectrometry. The validity of the methodology was checked by using the certified human hair material (BCR 397) and lyophilized human blood (Clincheck). The results indicated the higher contents of Pb in biological samples of indoor and outdoor mining workers than referents. However, the levels of Ca were found to be lower in indoor and outdoor mining workers than those of referents. It can be concluded that immediate action should be taken by recommended authorities to improve the ventilation and hygiene practices inside the industries, mines, and other workplaces.
文摘<strong>Background:</strong> Recently, Coronavirus Disease 2019 (COVID-19) has been affected by the extreme acute respiratory syndrome coronavirus 2 (SARS-CoV-2) and has developed important global health anxiety. At this time, the treatment options for this disease are only moderately successful. Smoking has been related to COVID-19 and its mortality, and it has the potential to affect bacteriological and viral conversion, clinical effects, and treatment outcomes. <strong>Methods:</strong> The aim of this study was to determine the relationship between critical essential trace {zinc (Zn), iron (Fe), and copper (Cu)} and toxic {cadmium (Cd) and nickel (Ni)} elements in human biological samples such as scalp hair, serum, saliva, blood, nasal fluid, and sputum of smoking and nonsmoking male COVID-19 patients (n = 139, age range 25 - 38 years) from Hyderabad, Pakistan. For comparative purposes, the biological specimens of referent persons (n = 83), pulmonary Tuberculosis (T.B) patients (n = 67), Pneumonia (n = 56) of the same age groups were also be analyzed. Microwave oven mediated digestion method was employed, and digestion of samples was carried out with the help of 2:1 mixture solution of HNO<sub>3</sub> (65%) and H<sub>2</sub>O<sub>2</sub> (30%). Atomic absorption spectrometry was employed for the determination of elemental concentrations from the microwave oven employed digested samples. <strong>Results:</strong> The found average of essential elements (Zn, Fe, and Cu) in biological specimens of smoker and nonsmoker male COVID-19, T.B, and Pneumonia patients was found to lower, whilst cadmium and nickel were found to be higher when compared with samples from referents (p < 0.001). <strong>Conclusions:</strong> Improved elemental (Cu, Fe, Zn) concentrations may also decrease the risk of bacterial co-infection by enhancing the mucociliary clearance and respiratory epithelial barrier function, in addition to providing direct antibacterial effects against <i>S. pneumoniae</i>. Our findings also suggest that higher Cd and Ni concentrations are linked to cigarette smoking, which could lead to COVID-19 and other lung-infected diseased recurrences. However, further clinical and experimental research is required.
基金supported by the National Natural Science Foundation of China(No.81102499)the Fundamental Research Funds for the Central Universities of Central South University and Hunan Science and Technology Project(No.2011SK3261)
文摘Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sample processing. To meet these emerging demands on biopharmaceutical analysis, this paper summarizes several new techniques of on-line biological sample processing: solid phase extraction, solid phase micro-extraction, column switching, limited intake filler, molecularly imprinted solid phase extraction,tubular column, and micro-dialysis. We describe new developments, principles, and characteristics of these techniques, and the application of liquid chromatography–mass spectrometry(LC–MS) in biopharmaceutical analysis with these new techniques in on-line biological sample processing.
基金supported by 973 Program (No. 2013CB933800) National Natural Science Foundation of China (Nos. 21390411, 21535004, 21422505, 21375081)Natural Science Foundation for Distinguished Young Scholars of Shandong Province (No. JQ201503)
文摘Ascorbic acid(AA) serves as a key coenzyme in many metabolic pathways. Enough daily AA supplements from different dietary sources are the only way for human to maintain their AA levels in body.Determination of AA content in different foods guides to build healthy diet, which is of great biomedical significance. Hence, developing a highly selective and instantaneous fluorescent nanoprobe for the detection of AA in biological samples is highly needed. Here we present a novel turn-on fluorescent nanoprobe using lanthanide-doped upconversion nanoparticles(UCNPs) and cobalt oxyhydroxide(Co OOH) nanoflakes for monitoring AA in fruit samples. In this nanosystem, the UCNPs can be adsorbed onto the Co OOH nanoflakes, leading to a remarkable fluorescence decrease through Fo?rster resonance energy transfer. Furthermore, the AA could trigger the disassembly of the Co OOH to liberate the upconverted fluorescence. The UCNPs-based nanoprobe can provide an effective platform for highly selective and rapid detection of AA in biological samples.
基金supported by Technology Project of Education Department in Fujian:A(JA14336).
文摘In order to control drug crime effectively,it is necessary to develop selective analytical methods suitable for unambiguous identification and determination of drugs in illicit samples and biological matrices.A novel microextraction technique based on ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction,(UA-LDS-DLLME)has been applied to the determination of four amphetamines(methamphetamine,amphetamine,3,4-methylenedioxymethamphetamine,and 3,4-methylenedioxyamphetamine)in urine samples by gas chromatography-mass spectrometry.The parameters affecting extraction efficiency have been investigated and optimized.UA-LDS-DLLME used ultrasound energy to assist in the emulsification process without any disperser solvent.Under the optimized conditions,linearity was observed for all analytes in the 0.15-10 p,g/mL range with correlation coefficients(R)ranging from 0.9886 to 0.9894.The recoveries of75.6-91.4%with relative standard deviations of 2.5-4.0%were obtained.The limits of detection(S/N=3)were estimated to be in the 5-10 ng/mL range.The UA-LDS-DLLME technique had the advantages of shorter extraction time,suitability for simultaneous pretreatments of batches of samples,and the higher extraction efficiency.It was successfully applied to the analysis of amphetamines in real human urine samples.
基金supported by the Health Institutes of Turkey(TüSEB)(Project No.2020CV01-8946)。
文摘A rapid,accurate,and sensitive analytical method,ultrasonication-assisted spraying based fine droplet formationeliquid phase microextractionegas chromatographyemass spectrometry(UA-SFDF-LPME-GCMS),was proposed for the determination of trace amounts of hydroxychloroquine sulfate in human serum,urine,and saliva samples.To determine the best extraction strategy,several liquid and solid phase extraction methods were investigated for their efficiencies in isolation and preconcentration of hydroxychloroquine sulfate from biological matrices.The UA-SFDF-LPME method was determined to be the best extraction method as it was operationally simple and provided accurate results.Variables such as the extraction solvent,spraying number,sodium hydroxide concentration and volume,sample volume,mixing method,and mixing period were optimized for the proposed method using the onevariable-at-a-time approach.In addition,Tukey’s method based on a post hoc comparison test was employed to evaluate the significant difference between the parameters inspected.After the optimization studies,the limit of detection(LOD)and limit of quantification(LOQ)were determined to be 0.7 and 2.4 mg/kg,respectively.The sensitivity of the GC-MS system based on the LOD was enhanced approximately 440-fold when the UA-SFDF-LPME method was employed.Spiking experiments were also conducted for the human serum,urine,and saliva samples to determine the applicability and accuracy of the proposed method.Recoveries for the human serum,urine,and saliva samples were found to be in the ranges of 93.9%-101.7%,95.2%-105.0%,and 93.1%-102.3%,respectively.These results were satisfactory and indicated that the hydroxychloroquine sulfate level in the above biological samples could be analyzed using the proposed method.
文摘A method was established for the analysis of omethoate and it’s concomitants and decomposed product in biological samples by GC-MS.This method is rapid,reliable and accurate.
文摘Objective:To assess the thorium exposure of the mine workers and the public to a typical rare earth mine and estimate the resultant committed effective dose to them.Methods:A total of 79 volunteers were selected in this survey,including 69 mine workers and 10 local residents living about 4 km away from the mine site.Urinary samples were collected from 79 volunteers,with 65 hair samples from 57 workers and 8 local residents.The thorium concentrations in urinary and hair samples were determined by using inductively coupled plasma mass spectrometry.The committed effective doses were estimated based on the urinary samples collected and the parameters as recommended by ICRP Publication 137.Results:Thorium concentrations in the samples from the workers ranged from 19.0 to 2388.8 ng/g in hair with median of 149.8 ng/g,and in urine 18.3–906.1 ng/L with median of 59.6 ng/L,respectively.The median values of thorium concentrations were 11.8 ng/g in hair and 32.40 ng/L in urine for the public respectively.The thorium concentrations in urinary and hair samples of the workers were not only higher than those of the residents in the local area,but also than those of non-occupationally exposed populations as reported.The median values of committed effective dose were estimated to be 1.51 mSv for the workers and 781μSv for the local residents,respectively.Conclusions:The residents in the local area,and especially the workers,have been subject to long term thorium exposure.More attention should be paid to the radiological hazards of thorium to the workers and local residents.