Analytical Methods
·
2016
·Vol. 8
·期 31
·6099-6106
·
IF 1.915
Lijun Qiao,Xiaohua Zhou,Yanhao Zhang,Ajuan Yu,Shusheng Zhang,Yangjie Wu
In this paper, a rapid and effective HPLC method, using a new 4-chloro-6-pyrimidinylferrocene-modified silica gel (NFcSi) as a solid-phase extraction (SPE) sorbent, was developed for the purification and determination of trace sulfonamides in foodstuffs. The main influencing factors of SPE including the amount of NFcSi sorbent, sample flow rate, and species and volume of the eluant were investigated and evaluated in a sample pretreatment step. The optimized purification effect was achieved at a sample flow rate of 2 mL min−1 with 100 mg of NFcSi and 5 mL of washing solution (water, 100%). The HPLC analysis was carried out on a Shim-Pack VP-ODS column (150 × 4.6 mm i.d., 5 μm) with a mobile phase of MeOH/0.1% acetic acid–water (30 : 70, v/v). With a detection wavelength of 270 nm, the good linearities of sulfadimidine (SM2), sulfamethoxazole (SMZ) and sulfadimethoxine (SDM) were obtained at concentrations ranging from 10 to 5000 ng mL−1 (R2 ≥ 0.9998). The RSD% values (n = 6) of retention times and peak areas in intra- and inter-day assays for three sulfonamides were all below 0.55%, 1.80%, 0.20% and 0.78%, which showed good precision. In addition, the overall recoveries of SM2, SMZ and SDM through the extraction and purification steps were in the range of 71.1–86.7%, 70.6–93.6% and 72.4–90.7%. Compared with commercial SPE sorbents, NFcSi featured excellent selectivity to retain polar and nonpolar interferents in sample matrices. The improved method was simple, rapid, accurate and promising for the determination of trace sulfonamides in foodstuffs with complex matrices.
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MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 4
·1161-1167
·
IF 4.58
Zhu Jianli,Chen Dongping,Ai Youhong,Dang Xueping,Huang Jianlin,Chen Huaixia
The authors have synthesized a dummy molecularly imprinted monolith (MIM) in the tip of a micropipette using a sol-gel method. The MIM was applied to selective solid-phase microextraction (SPME) of vanillin (VN) and methyl vanillin (MV) prior to their determination by HPLC. The MIM was characterized by thermogravimetric analysis, scanning electron microscopy and FTIR. Some parameters affecting SPME were optimized. Then, a sensitive SPME/HPLC method was developed for the determination of VN and MV in infant milk powder. Under optimized conditions, the response is linear in the 2 to 3000 μg∙kg −1 VN concentration range and in the 3 to 2000 μg∙kg −1 range for MV. The detection limits (for an S/N ratio of 3) are 0.5 and 1 μg∙kg −1 , and the recoveries are between 83 and 110% for VN and between 80 and 101% for MV.
A dummy molecularly imprinting monolith was synthesized and applied for SPME of vanillin and methyl vanillin before HPLC. The detection limits of the method for vanillin and methyl vanillin in milk powder were 0.5 and 1 μg·kg −1 , respectively.
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JOURNAL OF SEPARATION SCIENCE
·
2013
·Vol. 36
·期 8
·1343-1348
·
IF 2.591
Qiuyun Wang,Yajin Xiong,Baozhu Lu,Jun Fan,Sheng Zhang,Shengrun Zheng,Weiguang Zhang
N -(2,4-dinitrophenyl)-proline and N -(2,4-dinitrophenyl)-serine were enantiomerically resolved on the BSA chiral stationary phase by HPLC in reversed-phase mode. Effects of chromatographic conditions on enantioseparation and elution order have been investigated in detail. For these two samples, reversal of enantiomer elution order was observed by changing buffer pH, the content of acetonitrile, or alcohol modifiers in mobile phase, which is firstly reported in the BSA chiral stationary phase studies. More interestingly, combined effect between buffer pH and the content of acetonitrile was also observed. In addition, coelution range of enantiomers varied along with the content of acetonitrile in mobile phase.
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Analytical Methods
·
2012
·Vol. 5
·期 2
·536-540
·
IF 1.547
Jianfei Xiong,Xiangyu Tang,Guangming Zhou,Zhuo Guan,Limin Wu
A simple method was proposed for simultaneous determination of chlorpyrifos and its hydrolysis and biodegradation product 3,5,6-trichloro-2-pyridinol (TCP) in soil samples. The analytes were extracted with ethyl acetate (EtOAc) under optimized pretreatment conditions such as the type, volume and pH of extraction solvent. Clean-up of the extract from soil was conducted by dispersive solid phase extraction (DSPE) using activated carbon as the adsorbent. High performance liquid chromatography with ultraviolet detection (HPLC-UV) was used for simultaneous determination of the two analytes. Under the optimized HPLC conditions, the limits of detection (LOD), obtained on signal-to-noise ratio (S/N) of 3, for chlorpyrifos and TCP were 0.0080 mg kg−1 and 0.0120 mg kg−1, respectively. Linear calibration curves were obtained in the range of 0.05–2.00 mg kg−1 and 0.03–2.00 mg kg−1 for chlorpyrifos and TCP, respectively. The spike recoveries from soil ranged from 89.4% to 114%, and the relative standard deviation (RSD) was in the range of 0.80%–14%.
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JOURNAL OF FOOD SCIENCE
·
2015
·Vol. 80
·期 11
·C2452
·
IF 1.696
Juan Wang,Lei Zhang,Dingqiang Xin,Yaling Yang
en This link goes to a English section pt This link goes to a English section A novel, simple and low cost through coating Fe 3 O 4 magnetic nanoparticles (MNPs) with decanoic acid were synthesized. The functionalized MNPs showed excellent dispersibility in aqueous solution and were applied to dispersive micro-solid-phase extraction (D-μ-SPE) followed by high performance liquid chromatographic analysis for 4 phthalate esters (PAEs) including benzyl butyl phthalate (BBP), dicyclohexyl phthalate (DCHP), di-n-butyl phthalate (DBP), and di-n-octyl phthalate (DNOP) from liquor samples. The extraction equilibrium is achieved in 1 min. The MNPs allow easy and rapid isolation of PAEs by using an external magnet, which can be reused 5 times. The 4 PAEs linear dynamic ranges were in the range of 5 to 1000 ng/mL and the correlation coefficients values were 0.9999. The limits of detection were in the range of 0.91 to 2.43 ng/mL. The influences of the adsorbent dosage and the use frequency of adsorbent, the adsorption time, the solution pH and ionic strength were investigated and optimized. The proposed method was used to determine of PAEs in liquor samples and recoveries between 88.9% and 105.4%, with the relative standard deviations were below 4.0%. Practical Application en This link goes to a English section pt This link goes to a English section The results from this study can attract the attention of countries in control of liquors’ quality.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2013
·
IF 2.487
Jian-Yao Wang,Hai-Long Wu,Yan-Mei Sun,Hui-Wen Gu,Zhi Liu,Ya-Juan Liu,Ru-Qin Yu
A novel strategy that combines the chemometrics method with high performance liquid chromatography with fluorescence detector (HPLC–FLD) was developed for the simultaneous determination of seven phenolic antioxidants in six kinds of oil samples. After a simple dilution step, oil samples can be directly injected into the detecting system and the data were measured in a short time with a chromatographic system operating in the gradient elution mode. Since the chromatographic and spectral peaks among interesting analytes and interferences were heavily overlapped, second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm which fully exploiting the second-order advantage was adopted. Successful resolution was obtained in the presence of different matrix interferences in different oil samples, and the developed approach allows the quantification of the antioxidants at levels found in edible vegetable oils, without the necessity of applying either preconcentration or extraction steps, moreover, a column washing is also not required. Meanwhile, the effectiveness and reproducibility of the proposed method were also validated by some statistical parameters like root mean squared error of prediction (RMSEP), limits of detection (LOD) and relative standard deviation (RSD). Then the proposed method was compared with several commonly selected methods in sample preparation, elution time and LOD.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2014
·
IF 2.694
Yunfang Li,Yu Chen,Chuying Xiao,Dan Chen,Yuxiu Xiao,Zhinan Mei
α-Amylase inhibitors play an important role in management of diabetes and obesity. In order to rapidly discover potent α-amylase inhibitors from medicinal plants, a ligands-screening method based on enzyme-immobilized magnetic nanoparticles integrated with HPLC was developed. Amine-terminated magnetic nanoparticles were prepared for the immobilization of α-amylase. Based on the affinity theory, the α-amylase-coated magnetic nanoparticles were employed to fish out the ligands from the extracts of Garcinia xanthochymus , and the elutes were examined by HPLC. As a result, three ligands were screened out. Isolation and identification were carried out subsequently. By analyzing the UV, MS and NMR spectra, they were identified as three biflavonoids including GB2a glucoside (2), GB2a (3) and fukugetin (4). The IC 50 values of the three compounds were also determined. The results suggest the proposed approach is efficient and accurate, and has great potential in rapid discovery of drug candidates from medical plants.
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BIOMEDICAL CHROMATOGRAPHY
·
2014
·Vol. 28
·期 10
·1325-1334
·
IF 1.662
Zhangxiao Peng,Yan Wang,Xue Gu,Xiaojie Guo,Chao Yan
A method based on high-performance liquid chromatography coupled with ultraviolet detection was developed for studying the pharmacokinetics of costunolide (Cos) and dehydrocostus lactone (Dehy) in rats after intravenous (i.v.) administration. Following i.v. administration, the maximum plasma concentrations of Cos and Dehy were observed to be 12.29 ± 1.47 and 5.79 ± 0.13 µg/mL, respectively. The bioavailability of Cos was larger than that of Dehy; however, the clearance and the volume of distribution of Dehy were much larger than those of Cos. An ultraperformance liquid chromatography/quadrupole time-of-flight mass spectrometry system with automated MS E (E represents collision energy) data analysis software (MetaboLynx TM ) was used to analyze and identify the metabolites of Cos and Dehy in vivo . Four metabolites of Cos and six metabolites of Dehy were discovered from the plasma, urine and feces of rats. The main metabolic pathway of Cos was phase II biotransformation, but the main metabolic pathways of Dehy was phase І biotransformation. Two sequential desaturations and N -acetylcysteine conjugation were the common metabolic pathways of Cos and Dehy in rats. This information may be useful for the further development of the two drug candidates. Copyright © 2014 John Wiley & Sons, Ltd.
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STEROIDS
·
2015
·
IF 2.639
Xinxin Zhang,Zengjun Guo,Jing Li,Yoichiro Ito,Wenji Sun
A specific high performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS method) was established for determining the concentration of protodioscin (PG) in rat plasma after intragastric administration of its standard form. Ginsenoside Rb 1 was selected as the internal standard (IS). The plasma sample was prepared using one-step deproteinization procedure by adding three parts of acetonitrile to precipitate proteins. The chromatographic separation was accomplished on an Inersil ODS-3 C 18 column (250 × 4.6 mm, 5 μm) with a mobile phase composed with acetonitrile and water containing 0.1% formic acid under a gradient elution mode at a flow rate of 1 mL min −1 . A 3:1 portion of the eluent after a microsplit was detected on a triple quadrupole tandem mass spectrometer coupled with electrospray ionization (ESI) in positive ion and multiple reaction monitoring (MRM) scanning modes. The mass transitions were selected as 888.1 → 1050.2 for PG and 948.2 → 1110.3 for IS, respectively. After careful validation, the plasma samples were always stable under different storage conditions. These analytical results rendered sensitive, selective, and reliable values by this established method which displayed high accuracy, adequate extracted recoveries, and almost negligible matrix effects. This method was applied to the pharmacokinetic studies on PG level in the rat plasma and its pharmacokinetic effect. The results of our studies suggest that the present method may be a useful tool for further clinical study of PG.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2017
·
IF 2.603
Shengfeng Huang,Ning Gan,Haibo Liu,You Zhou,Yinji Chen,Yuting Cao
In this work, a novel aptamer functionalized magnetic adsorbent was developed and combined with magnetic dispersive solid phase extraction (MDSPE) for selective enrichment of several amphenicol antibiotics residues (chloramphenicol(CAP), thiamphenicol(TAP) and florphenicol(FF)) in foodstuff then determined by High Performance Liquid Chromatography (HPLC)-Diode array detector(DAD). Firstly, a magnetic silica-coated Fe 3 O 4 microsphere(Fe 3 O 4 @SiO 2 ) was synthetized by sol-gel method, then it was functionalized by amino groups through 3-Aminopropyltriethoxysilane (APTES) reagent to form Fe 3 O 4 @SiO 2 -NH 2 ; Thirdly, the amino group on Fe 3 O 4 @SiO 2 -NH 2 was transferred to carboxylic group via the succinic anhydride to form Fe 3 O 4 @SiO 2 -COOH. Finally a kind of DNA aptamer with amino group which can simultaneously recognize CAP, TAP, FF, was functionalized on Fe 3 O 4 @SiO 2 -COOH through adding the EDC/sulfo-NHS coupling reagent (Fe 3 O 4 @SiO 2 @Apt). Therefore, a very stable and useful adsorbent was synthesized for the detection of chloramphenicol series antibiotics. This adsorbent can specifically and simultaneously recognize and enrich CAP, TAP, and FF with high adsorption amount from some complicated food matrix, e.g. milk based on the high affinity of aptamer towards the analytes. The saturated extraction capacities for CAP, TAP and FF by the adsorbent were 2.82, 2.56, 2.72 μg/g (mass of target/adsorbent)respectively and the enrichment folds were more than 100 times. Afterwards, the target analytes were washed away by pH 8.5 0.1 M Tris-HCl buffer solution and detected by HPLC-DAD. The parameters including extraction temperature, extraction capacity, extraction & desorption pH, extraction & desorption time were investigated. With the optimized conditions, the limits of detection (LOD) and limits of quantitation (LOQ) were 0.12–0.17 ng/ml and 0.40–0.55 ng/ml for the amphenicols in milk. The adsorbent also has good reproducibility for extraction which can be reused at least for 60 cycles with the recovery over 80% (Fig. S2). The MDSPE combined with HPLC-DAD detection possessed the advantages of high selectivity, extraction capacity and very convenient for magnetic separation. In addition, this method is environment friendly and employed no organic solution in the period of pretreatment and extracting. It is a universal platform which can be extended to selective enrichment other organic pollutants residues if changing the modified aptamers.
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Food Chemistry-X
·
2025
·
IF 8.2
Mengdie Cai,Xinyu Wang,Kun Lu,Bixiao Zhou,Lijun Wei,Xianglei Cheng
Residues of nitro-containing drugs in food and the environment have aroused social concern because of their excessive use for the treatment of human and animal diseases. The disadvantages of complex and time-consuming pretreatments in existing methods make it imperative to develop novel methods. Herein, with the aid of recognition probe MCLA, an excellent selective method for the detection of nitroimidazoles (NDZs) was developed based on high-performance liquid chromatography combined with ultraviolet (UV) degradation and chemiluminescence (HPLC-UV-CL). The study proposed an innovative process for the formation of SO 4 •− , •OH, and •NO via advanced oxidation processes of NDZs. Six studied NDZs achieved baseline separation within 24 min with detection limits as low as 3 ng/mL (S/N = 3 ). The proposed method is efficient, cost-effective, and does not require complicated purification steps. This study presents a unique approach for the detection of nitro-containing contaminants and provides new insights into monitoring advanced oxidation processes.
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MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Wenqing Zhang,Hao Zhu,Wenjie Xie,Chuanyuan Du,Xiuqiang Fang,Ruiming Zhang,Xiaosong Hu,Yawei Lin
A novel fluorescent probe , 3-(4-((hydroxylamino)methyl)-1H-pyrazol-1-yl)-7-methoxyl coumarin (HAPMC), has been designed and synthesized. The compound exhibits exceptional fluorescence properties due to a coumarin-pyrazolyl fluorophore. Moreover, it incorporates an N -hydroxylamine functional group capable of reacting with aldehydes to yield nitrone derivatives under mild conditions. This unique combination renders it an ideal derivatization reagent for aldehyde analysis. A standard method was established for the quantitative analysis of eight fatty aldehydes by utilizing high-performance liquid chromatography with fluorescence detection (HPLC-FLD) and a pre-column derivatization process, which has low detection limits (0.3–1.2 nM), satisfactory reproducibility (intraday and interday relative standard deviations in the range of 1.29 %-2.92 % and 1.73 %-3.45 %), and an extensive linear range (25–5000 nM) with excellent linearity (R 2 ≥ 0.9989). The spiked recoveries of the fatty aldehydes range from 89.6 % to 106.0 %. The greenness and sustainability of our approach are reinforced by evaluations conducted with the AGREE and RGB 12 algorithms. The established method was successfully applied to the qualitative and quantitative detection of fatty aldehydes in nine real vegetable oil samples, including peanut, canola, rice, soybean, olive, rapeseed, corn, sunflower, and blended oils. The fatty aldehydes are known to have adverse effects on human health due to their carcinogenic and mutagenic properties. The findings revealed that hexanal and nonanal were the most prevalent saturated fatty aldehydes, with a notable increase in the total aldehyde concentration observed as the temperature and duration of heating increased. Compared to alternative analytical techniques, this pre-column derivatization method utilizing HAPMC displayed simplicity, reliability, and sensitivity. The results demonstrate the potential for broad application of this approach in various important research domains, including food quality control, environmental monitoring, and medical research.
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