JOURNAL OF SEPARATION SCIENCE
·
2020
·Vol. 43
·期 17
·3499-3508
·
IF 2.878
Yinan Guo,Wei Wei,Ying Zhang,Yuanyuan Dai,Weiping Wang,Aijun Wang
An aptamer (Apt) functionalized magnetic material was prepared by covalently link Apt to Fe 3 O 4 /graphene oxide (Fe 3 O 4 /GO) composite by 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride and N -hydroxysuccinimide, and then characterized by FTIR spectroscopy, X-ray diffraction, and vibration sample magnetometry. The obtained composite of Fe 3 O 4 /GO/Apt was employed as magnetic solid-phase extraction adsorbent for the selective preconcentration of sulfadimethoxine prior to analysis by high-performance liquid chromatography. Under the optimal conditions (sample pH of 4.0, sorbent dosage of 20 mg, extraction time of 3 h, and methanol-5% acetic acid solution as eluent), a good linear relationship was obtained between the peak area and concentration of sulfadimethoxine in the range of 5.0 to 1500.0 µg/L with correlation coefficient of 0.9997. The limit of detection ( S/N = 3) was 3.3 µg/L. The developed method was successfully applied to the analysis of sulfadimethoxine in milk with recoveries in the range of 75.9-92.3% and relative standard deviations less than 8.1%. The adsorption mechanism of Fe 3 O 4 /GO/Apt toward sulfadimethoxine was studied through the adsorption kinetics and adsorption isotherms, and the results show that the adsorption process fits well with the pseudo-second-order kinetic model and the adsorbate on Fe 3 O 4 /GO/Apt is multilayer and heterogeneous.
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高影响因子
EUROPEAN FOOD RESEARCH AND TECHNOLOGY
·
2020
·Vol. 246
·期 10
·1909-1918
·
IF 2.366
Zhang Xiao-Hua,Ma Yi-Xin,Yi Chong,Qing Xiang-Dong,Liu Zhi,Zheng Jing-Jing,Lin Fang,Lv Tian-Feng
In this paper, the application of chemometrics coupled with high-performance liquid chromatography-diode array detection (HPLC–DAD) for the rapid and sensitive quantitative analysis of seven flavonoids in the raw and purified propolis samples was investigated. The objective of this paper was to receive a successful resolution of the complex propolis matrix with minimum experimental time (3.5 min) when appearing unknown interferences, highly overlapping peaks, time and baseline drifts among chromatograms. First, the validation samples contained seven flavonoids at five levels, helped to understand and interpret the features of the second-order calibration method based on the alternating trilinear decomposition (ATLD) algorithm. Second, the experimental data were studied for the simultaneous determination of flavonoids in the raw and purified propolis samples using the function of "mathematical separation" of ATLD algorithm. Except for myricetin (MY), the average recoveries of other analytes were 95.79–105.82% for the raw propolis samples, 94.41–108.06% for the purified propolis samples. In addition, the limit of detection (LOD, 0.01–0.20 μg mL −1 ), limit of quantification (LOQ, 0.03–0.60 μg mL −1 ), sensitivity (SEN, 15.97–184.31 mL μg −1 ), selectivity (SEL, 0.16–0.76) and root-mean-squared error of prediction (RMSEP, 0.29–1.64 μg mL −1 ) of the proposed method, demonstrated that all the target analytes have good sensitivity, low detection limit. According to the experimental results, the total content of flavonoids in purified propolis is about twice that in raw propolis, which is consistent with the actual situation. This analytical strategy will be extremely promising for the identification and quantification of analytes studied in the complex samples.
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高影响因子
CHROMATOGRAPHIA
·
2021
·Vol. 84
·期 11
·1057-1064
·
IF 2.044
Zhang Hanzhi,Li Feng,Dun Junling,Sun Ning,Liu Hao,Chen Guiliang
An analysis strategy that can simultaneously determine the amino acid site information and configuration for polymyxin (PM) components is reported in this study. The main components of PMB1, PMB2, and PMB1-I (the Leucine at position 7 changed to be Isoleucine) were purified from the mixture of PMB. The PMB component was hydrolyzed by hydrochloric acid to be a mixture of amino acids, which were derivatized with Marfey’s reagent of N α -(5-fluoro-2,4-dinitrophenyl)- l -alanine amide ( l -FDAA), and then, the configurations of amino acids were easily determined by HPLC–MS. However, the aforementioned method could not offer the information of amino acid at each site, a specific enzymatic hydrolysis method combined Edman degradation was developed. The fatty acyl-diaminobutyric acid (position 1) of PMB component was removed by ficin, and the PMB components were transformed to be PMB nonapeptide. The amino acids at each site of the nonapeptide were determined by N-terminal sequencing. Combining the results of the above methods, the amino acid information and configuration of each site in PM components can be determined, especially the l -Leucine and l -Isoleucine in PMB1 and PMB1-I. The workflow was useful for other PM analogues to identify the sequence and configuration for quality control.
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高影响因子
PREPARATIVE BIOCHEMISTRY & BIOTECHNOLOGY
·
2021
·
IF 2.162
Guilong Yan,Yuzhen Zhou,Yonghong Hu,Liqin Zhao,Wei Wang
Counter-current chromatography (CCC) target-guided by on-line HPLC with post-column DPPH assay was established for efficient screening and isolation of large amount of antioxidants from Eupatorium lindleyanum DC. On-line HPLC with post-column DPPH reaction was used to screen the antioxidants and optimize the biphasic solvent system of CCC, then the targeted peaks were purified using CCC. In the present study, three compounds, nepetin, cirsiliol and jaceosidin, were targeted and successively separated from n-butanol fraction of E. lindleyanum DC. by this strategy. All three compounds showed strong DPPH radical scavenging activity. These results confirmed that the strategy would be an efficient and effective method to isolate antioxidants from complex mixtures.
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JOURNAL OF SEPARATION SCIENCE
·
2021
·Vol. 44
·期 20
·3777-3788
·
IF 3.645
Ping Zhang,Zeli Chun,Qiju Shao,Lidan Fu,Yipan Luo,Ding Gu,Rongxiang Chen
A combinative method using high-performance liquid chromatography-electrochemical detection for fingerprinting and quantitative analysis was developed and successfully applied for the quality evaluation of Lophatherum gracile Brongn leaves collected from 21 geographical locations in China. In the fingerprint analysis, 18 common peaks were observed among the 21 samples, and 10 peaks were identified. Simultaneous quantification of the 10 components was conducted to interpret the variations in these compounds among the L. gracile Brongn leaves originating from different geographical locations. The correlation between the chromatograms and the antioxidant activities of the samples was further studied. The results indicated a linear correlation between the antioxidant activity and the total common peak areas of the fingerprints obtained by high-performance liquid chromatography-electrochemical detection. Importantly, it was found that high-performance liquid chromatography-electrochemical detection fingerprinting can not only determine the quantities of individual components present in such samples but also evaluate the antioxidant activities of the samples. The developed method is a valuable reference for the further study and development of L. gracile Brongn.
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JOURNAL OF FOOD SCIENCE
·
2019
·Vol. 84
·期 12
·3624-3633
·
IF 2.081
Chunyan Tu,Yinan Guo,Yuanyuan Dai,Wei Wei,Weiping Wang,Liang Wu,Aijun Wang
An aptamer-functionalized Fe 3 O 4 /graphene oxide was synthesized by chemical co-precipitation method and then employed in the magnetic solid-phase extraction for selective enrichment of chloramphenicol before HPLC. The aptamer was covalently bonded to the Fe 3 O 4 /graphene oxide complex by 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride and N -hydroxysuccinimide. Parameters affecting extraction efficiency including solution pH, extraction time and temperature, types and volume of elution solvent, and elution time were investigated in detail. Under the optimal conditions, good linearity was obtained between the peak area and analyte concentration in the range of 7.0 to 1.0 × 10 3 µg/L with the correlation coefficient of 0.9994. The limit of detection and quantitation were 0.24 µg/L and 0.79 µg/L, respectively. The developed method was employed to the analysis of chloramphenicol in honey and milk samples. The recoveries ranged from 80.5% to 105.0% with relative standard deviations less than 8.9%. Practical Application An aptamer-functionalized Fe 3 O 4 /graphene oxide was synthesized and employed in magnetic solid phase extraction for the enrichment of chloramphenicol before HPLC. The presented assay was employed for the determination of chloramphenicol in honey and milk with satisfactory results.
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高影响因子
TALANTA
·
2019
·
IF 4.916
Xing Huang,Dan Xiao,Yanli Tong,Zuanguang Chen
High performance liquid chromatography (HPLC) post-column photochemical reaction (PR) coupled capacitively coupled contactless conductivity detector (C 4 D) was used for the first time in analysis of weak ultraviolet (UV)-absorbing, non-fluorescence and nonpolar compound. A series of conditions including the radiation power of light source, the length of the reaction tube and the thickness of detection tube were investigated. HPLC-PR-C 4 D system was successfully applied to the determination of Cyclosporin A (CsA). Consequently, under optimal conditions, the detection system exhibited a detection limit of 0.04 μg/mL and wide linear range from 0.5 μg/mL to 100 μg/mL for CsA detection. Application of the HPLC-PR- C 4 D system to pharmaceutical formulation and biological samples revealed the system developed maybe reliably applied to clinical studies.
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高影响因子
Separation Science Plus
·
2018
·Vol. 1
·期 5
·367-373
·
IF 0
Xuemei Wang,Huan Wang,Pengfei Huang,Xiaomin Ma,Xinzhen Du,Xiaoquan Lu
A specific, precise and accurate high-performance liquid chromatography method with ultraviolet detection was established for the simultaneous determination of eight insecticides in fruit samples. Samples were extracted with acetone and cleaned using the quick, easy, cheap, effective, rugged, and safe technique. Under the optimized conditions, wide linearity ranges (5.0–2000 μg kg −1 ) were obtained for the eight insecticides and the correlation coefficients ( r ) ranged from 0.9985 to 0.9994. The limit of detection and limit of quantification were 0.27–1.85 and 0.90–6.18 μg kg −1 , respectively, and acceptable reproducibility (RSD < 6.6% for intra-day, < 9.2% for inter-day) were achieved. The recovery rates for all insecticides at two spiked levels of 20 and 50 μg kg −1 in fruits samples ranged from 85.9 to 110.4%, and the relative standard deviations were in the range of 3.3–8.9%. The results demonstrated clearly that the approach developed provides reliable, simple, rapid and environmentally friendly quantification and identification of eight insecticides in fruits. These results not only gave insights about the insecticides but also contributed to environmental protection and food safety.
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MOLECULES
·
2018
·Vol. 23
·期 8
·2045
·
IF 3.098
Ying Nie,Weifeng Yao
The quantitative analysis of multiple indexes remains an important quality evaluation method of traditional Chinese medicine (TCM) herbal formulas. The Chinese Pharmacopoeia 2015 only stipulates the content of a single component, specnuezhenide, in Erzhiwan composed of the Fructus Ligustri Lucidi (FLL) powder and aqueous extracts of Herba Ecliptae (HE). To generalize the intrinsic quality of Erzhiwan, a novel C30-HPLC method with good precision, accuracy, and reproducibility was developed for the simultaneous determination of six compounds, including two isomers, and then an analytic hierarchy process was further applied to integrate and discriminate the quality of four samples prepared via different methods. The results of the analysis were in agreement with the antioxidant tests in vitro. This comprehensive strategy could provide a reference and suggestions for the improvement of the quality evaluation method of TCM herbal formulas.Keywords:analytic hierarchy process;C30-HPLC;Erzhiwan;herbal formula;quality evaluation
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Analytical Methods
·
2018
·Vol. 10
·期 46
·5577-5588
·
IF 2.073
Qian Liu,Hai-Long Wu,Zhi Liu,Rong Xiao,Tong Wang,Yong Hu,Yu-Jie Ding,Ru-Qin Yu
A methodology for simultaneously measuring seventeen polyphenols in six Chinese raw propolis samples by using chemometrics-assisted high performance liquid chromatography-diode array detection (HPLC-DAD) was developed and validated. With the aid of a second-order calibration method based on an alternating trilinear decomposition (ATLD) algorithm, HPLC analysis was easily achieved within 16.5 min even in the presence of heavily overlapped peaks and unknown interferents. The average recoveries were in the range of 95.2% to 118.7% with standard deviation less than 7.0% for the selected raw propolis. Figures of merit including sensitivity (SEN), selectivity (SEL), root mean square errors of prediction (RMSEPs), etc. were calculated to validate the accuracy of the proposed method. For further confirmation, a multiple reaction monitoring (MRM) method based on LC-MS/MS was adopted. The paired F-test and t-test results showed that there was no significant difference between the MRM and the proposed method at the 95% confidence level, which indicated that the developed ATLD-assisted HPLC-DAD method is a suitable tool for the rapid analysis of Chinese raw propolis. Considering its advantages of simplicity, rapidity, precision and accuracy, it might also be extended as an alternative and available method for the quality monitoring of propolis raw material in the pharmaceutical industry.
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FOOD CHEMISTRY
·
2012
·
IF 3.655
Xiao-Hua Zhang,Hai-Long Wu,Jian-Yao Wang,De-Zhu Tu,Chao Kang,Juan Zhao,Yao Chen,Xiao-Xia Miu,Ru-Qin Yu
This paper describes the use of second-order calibration for development of HPLC-DAD method to quantify nine polyphenols in five kinds of honey samples. The sample treatment procedure was simplified effectively relative to the traditional ways. Baselines drift was also overcome by means of regarding the drift as additional factor(s) as well as the analytes of interest in the mathematical model. The contents of polyphenols obtained by the alternating trilinear decomposition (ATLD) method have been successfully used to distinguish different types of honey. This method shows good linearity ( r > 0.99), rapidity ( t < 7.60 min) and accuracy, which may be extremely promising as an excellent routine strategy for identification and quantification of polyphenols in the complex matrices.
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JOURNAL OF SEPARATION SCIENCE
·
2013
·Vol. 37
·期 5
·587-594
·
IF 2.591
Ting Yang,Chao Ma,Huaixia Chen,Yajie Zhang,Xueping Dang,Jianlin Huang
An IPC-imprinted (IPC is isoprocarb) poly(methacrylic acid)/SiO 2 hybrid monolithic column was prepared and applied for the recognition of the template. The hybrid monolithic column was synthesized in a micropipette tip using methyltrimethoxysilane as the inorganic precursor, 3-(methacryloxy)propyltrimethoxysilane as the coupling agent, and ethylene glycol dimethacrylate as the cross-linker. The synthesis conditions, including the porogenic solvent, coupling agent, volume ratio of the inorganic alcoholysate and organic part, were optimized. The prepared monolithic column was characterized by SEM and FTIR spectroscopy. A simple, rapid, and sensitive method for the determination of IPC in rice using the imprinted monolithic column microextraction combined with HPLC was developed. Several parameters affecting the sample pretreatment were investigated, including the eluent, washing solution, and loading sample volume. The linearity of the calibration curve was observed in the range of 9.0–1000 μg/kg for IPC in rice with the correlation coefficient ( r 2 ) of 0.9983. The LOD was 3.0 μg/kg (S/N = 3). The assay gave recovery values ranging from 91 to 107%. The proposed method has been successfully applied for the selective extraction and sensitive determination of IPC in rice and a satisfactory result was obtained.
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高影响因子
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