Monolithic silica spin column extraction(MonoSpin-SPE)was developed as a simple,sensitive,and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry(UFLC-MS)to determin...Monolithic silica spin column extraction(MonoSpin-SPE)was developed as a simple,sensitive,and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry(UFLC-MS)to determine the levels of six phthalate esters,dimethyl-(DMP),diethyl-(DEP),dipropyl-[DPrP],butyl-benzyl-(BBP),dicyclohexyl-(DcHP),and di-n-octyl-(DOP)phthalate in physiological saline samples.Under optimized experimental conditions,the method was linear in the following ranges:0.2-50 μg/L for DMP,DEP,DPrP,DcHP and DOP;5-100 μg/L for BBP.The correlation coefficients(R2)were in the range of 0.9951-0.9995 for all the analytes and the limits of detection(LODs)and limits of quantification(LOQs)were in the ranges of 0.02-0.9 μg/L and 0.08-2.7 μg/L,respectively.The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations(RSDs)below 8.5% and 11.2%,respectively.This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%.DMP and DEP were found in actual physical saline samples(brand A and brand B).展开更多
A method of on-line pretreatment coupled to HPLC with fluorescence detection was developed and validated for the determination of nine quinolones in honey samples. This method simplified the complicated process of sam...A method of on-line pretreatment coupled to HPLC with fluorescence detection was developed and validated for the determination of nine quinolones in honey samples. This method simplified the complicated process of sample pretreatment and reduced sample treatment time. Recovery of the quinolones was between 92% - 101% for spiked honey samples. The limit of detection was 0.22 - 3.78 ng/mL (signal/noise ratio = 3). There was good linear correlation between HPLC peak area and concentration of the quinolones, with a linear range of 1.0 - 100.0 ng/mL and correlation coefficients >0.9997. The method proposed was validated for detecting quinolones in honey samples.展开更多
Chloramphenicol is an antibiotic and one of the potential contaminants in honey.Solid-phase extraction is the key pretreatment procedure for analysis of chloramphenicol in honey.In this work,an on-line pretreatment li...Chloramphenicol is an antibiotic and one of the potential contaminants in honey.Solid-phase extraction is the key pretreatment procedure for analysis of chloramphenicol in honey.In this work,an on-line pretreatment liquid chromatography-tandem mass spectrometer system for sensitive,reliable and higher throughput analysis was developed.With the methylcellulose-immobilized reversed-phase column,sugars in a honey sample were efficiently removed in 1 min.As a result,the limit of quantitation of chloramphenicol was 20 pg/mL(0.2 μg/kg honey).展开更多
A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separat...A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separation of some fat-soluble components in foods. Three columns including a trap column,concentration column and analytical column were used for trapping the fat-soluble components, on-line enrichment and reverse phase separation, respectively. Capsaicinoids were on-line extracted by a CO_2 supercritical fluid, then concentrated and separated by using the C_(18) columns, finally detected by mass spectrometry(MS). Capsaicin eluted at 10.1 min and limit of detection(LOD, S/N=3) for the standard solution is 0.55pg. The linearity was calculated with a value of coefficient of determination(R^2)≥0.998 in the range of 1.1–8.5 ng. Concentrations of capsaicin in the green, yellow, and red bell peppers were determined to be 60.33 ng/g, 31.79 ng/g, 35.38ng/g, respectively.展开更多
基金supported by the National Natural Science Foundation of China(Nos.90813015,20935002)
文摘Monolithic silica spin column extraction(MonoSpin-SPE)was developed as a simple,sensitive,and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry(UFLC-MS)to determine the levels of six phthalate esters,dimethyl-(DMP),diethyl-(DEP),dipropyl-[DPrP],butyl-benzyl-(BBP),dicyclohexyl-(DcHP),and di-n-octyl-(DOP)phthalate in physiological saline samples.Under optimized experimental conditions,the method was linear in the following ranges:0.2-50 μg/L for DMP,DEP,DPrP,DcHP and DOP;5-100 μg/L for BBP.The correlation coefficients(R2)were in the range of 0.9951-0.9995 for all the analytes and the limits of detection(LODs)and limits of quantification(LOQs)were in the ranges of 0.02-0.9 μg/L and 0.08-2.7 μg/L,respectively.The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations(RSDs)below 8.5% and 11.2%,respectively.This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%.DMP and DEP were found in actual physical saline samples(brand A and brand B).
文摘A method of on-line pretreatment coupled to HPLC with fluorescence detection was developed and validated for the determination of nine quinolones in honey samples. This method simplified the complicated process of sample pretreatment and reduced sample treatment time. Recovery of the quinolones was between 92% - 101% for spiked honey samples. The limit of detection was 0.22 - 3.78 ng/mL (signal/noise ratio = 3). There was good linear correlation between HPLC peak area and concentration of the quinolones, with a linear range of 1.0 - 100.0 ng/mL and correlation coefficients >0.9997. The method proposed was validated for detecting quinolones in honey samples.
基金supported by the National Natural Science Foundation of China(No.21227006)the Research Fund for the Doctoral Program of Higher Education(No.20110002110052)
文摘Chloramphenicol is an antibiotic and one of the potential contaminants in honey.Solid-phase extraction is the key pretreatment procedure for analysis of chloramphenicol in honey.In this work,an on-line pretreatment liquid chromatography-tandem mass spectrometer system for sensitive,reliable and higher throughput analysis was developed.With the methylcellulose-immobilized reversed-phase column,sugars in a honey sample were efficiently removed in 1 min.As a result,the limit of quantitation of chloramphenicol was 20 pg/mL(0.2 μg/kg honey).
基金supported by the National Natural Science Foundation of China (No. 21621003)
文摘A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separation of some fat-soluble components in foods. Three columns including a trap column,concentration column and analytical column were used for trapping the fat-soluble components, on-line enrichment and reverse phase separation, respectively. Capsaicinoids were on-line extracted by a CO_2 supercritical fluid, then concentrated and separated by using the C_(18) columns, finally detected by mass spectrometry(MS). Capsaicin eluted at 10.1 min and limit of detection(LOD, S/N=3) for the standard solution is 0.55pg. The linearity was calculated with a value of coefficient of determination(R^2)≥0.998 in the range of 1.1–8.5 ng. Concentrations of capsaicin in the green, yellow, and red bell peppers were determined to be 60.33 ng/g, 31.79 ng/g, 35.38ng/g, respectively.
