Co-reporter:Junfeng Zhu, Xiaojiao Yi, Peng Huang, Shuqing Chen, Yongjiang Wu
Journal of Pharmaceutical and Biomedical Analysis 2017 Volume 134() pp:100-107
Publication Date(Web):5 February 2017
DOI:10.1016/j.jpba.2016.11.028
•Ultrafiltration LC–MS combined with molecular modeling was developed to investigate the drug-protein binding of DHI.•Seven compounds in DHI were identified as HSA ligands.•The influence of aspirin on the DHI-HSA binding was investigated by competitive binding assay.Danhong injection (DHI) is a widely used Chinese medicine injection (CMI) for the clinical treatment of cardiovascular and cerebrovascular diseases. In this study, a simple and efficient in vitro method based on ultrafiltration LC–MS and molecular modeling has been developed to study the human serum albumin (HSA) binding of the compounds in DHI. Seven major components including protocatechuic aldehyde, p-coumaric acid, salvianolic acid D, rosmarinic acid, salvianolic acid E, lithospermic acid and salvianolic acid B were identified as HSA ligands and their binding degrees in the proposed non-saturated model were 26.17, 37.69, 99.77, 91.78, 96.91, 99.42 and 98.10%, respectively. Considering the drug-HSA binding property of the compounds in DHI may change during drug combination therapy, competitive binding assay was carried out to evaluate the influence of aspirin on the DHI-HSA binding. Experimental results revealed that the salvianolic acids in DHI had stronger binding ability to HSA than sodium salicylate. To further verify the results above, molecular modeling and probe displacement assay were conducted to investigate the optimum binding site and binding affinity of the ligands on HSA. Our findings suggested that the established method could be a powerful tool to study the drug-HSA binding property of CMIs.
Co-reporter:Peng Huang, Qing Zhang, Hongye Pan, Lianjun Luan, Xuesong Liu, Yongjiang Wu
Separation and Purification Technology 2017 Volume 175() pp:203-212
Publication Date(Web):24 March 2017
DOI:10.1016/j.seppur.2016.11.031
•An efficient process was applied for extraction and enrichment of total flavonoids from Scutellariae barbatae herba.•BBD experimental design was conducted for optimizing three parameters.•High quality of total flavonoids were obtained through the integrated process.In the present study, integrated extraction-adsorption process was developed and applied to extract and purify total flavonoids from Scutellariae barbatae herba. Screening of macroporous resins, single factor experiments, an experimental design based on Box-Behnken design (BBD) and purification conditions study were carried out to optimize the integrated process. DM130 resin was chosen as adsorbent and the optimal extraction-adsorption conditions were determined as pH of extraction solvent 2, time 9 h, liquid/solid ratio 20:1 mL/g and flow rate 7 BV/h. 70% (5 BV) ethanol aqueous solution was selected as elution solvent. Through this procedure, the total flavonoids of Scutellariae barbatae herba can be totally extracted using water as extraction solvent rather than high concentration ethanol was used in traditional extraction method. Moreover, the integrated process can simplify operation, reduce energy consumption, and prevent the degradation of bioactive substances, thus improve the quality of products. Compared to the conventional method, the recovery yield and purity of total flavonoids obtained from this procedure increased by 1.50 and 1.16 times respectively. The results showed that the integrated procedure can be efficient and eco-friendly, as well as appropriate for large-scale extraction and purification of total flavonoids from Scutellariae barbatae herba.
Co-reporter:Junfeng Zhu, Xiaojiao Yi, Wenhui Liu, Yingchun Xu, Shuqing Chen, Yongjiang Wu
Talanta 2017 Volume 165() pp:508-515
Publication Date(Web):1 April 2017
DOI:10.1016/j.talanta.2016.12.089
•A novel affinity selection combined with LC/MS approach was developed for multicomponent screening.•The proposed screening method is time- and cost-effective, easily recycled, and high-throughput.•Isochlorogenic acid A in Dendranthema indicum flowers was identified as a PPARγ ligand for the first time.Screening agonists of peroxisome proliferator-activated receptor-γ (PPARγ) from natural products is particularly motivated by the need for effective anti-diabetic agents. However, method for direct identification of PPARγ ligands from a complex sample is rarely reported. Here we propose a novel immobilized fusion protein affinity chromatography (IFPAC) to achieve rapid multicomponent screening. First, functional human PPARγ ligand binding domain (hPPARγLBD) was bacterially produced by fusion to glutathione S-transferase (GST). The unpurified GST-hPPARγLBD was directly applied to a 96-well filter plate prepacked with glutathione sepharose. Due to the strong affinity between GST and glutathione, the fusion protein could selectively attach to the glutathione matrix with an oriented immobilization, which was rapidly purified under non-denaturing conditions. Experimental results indicated that the prepared 96-affinity column array exhibited excellent selectivity and sensitivity for fishing novel interacting compounds. The proposed approach was applied in the high-throughput screening of PPARγ ligands from natural products, followed by rapid characterization of active compounds using HPLC–ESI-Q-TOF-MS/MS. Isochlorogenic acid A in Dendranthema indicum flowers was found to be a PPARγ ligand. Our findings suggested the IFPAC could be a powerful tool for drug discovery from natural products.
Co-reporter:Junfeng Zhu, Xiaojiao Yi, Jinghui Zhang, Shuqing Chen, Yongjiang Wu
Journal of Chromatography B 2017 Volume 1060(Volume 1060) pp:
Publication Date(Web):15 August 2017
DOI:10.1016/j.jchromb.2017.06.022
•A total of 127 compounds in YXST were successfully identified by HPLC–ESI-Q-TOF-MS/MS.•The antioxidant activity of YXST was investigated and the potential antioxidants were rapidly screened by DPPH-HPLC assay.•The in vivo antioxidants of YXST were screened and their antioxidant activity was assessed by DPPH spectrophotometric assay.Yangxinshi Tablet (YXST) is a Chinese patent medicine commonly used to treat cardiovascular diseases. However, its detailed chemical basis and mechanisms of action have not been clarified. In this study, high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (HPLC–ESI-Q-TOF-MS) was applied for comprehensive analysis of the chemical constituents in YXST. A total of 127 compounds, including 19 phenolic acids, 12 alkaloids, 51 flavanoids, 32 triterpenoids, 2 lignans, 2 phenylethanoid glycosides, 2 anthraquinones, 1 coumarin, and 6 other compounds, were identified or tentatively deduced by comparing their retention times and MS spectra with those of authentic standards or literature data. To further prove the antioxidant activity of YXST, its free radical scavenging capacity was assessed by 1,1-diphenyl-2-picrylhydrazyl (DPPH) spectrophotometric assay and the antioxidants in YXST were rapidly screened by DPPH-HPLC experiment. Especially, salvianolic acid A and salvianolic acid B showed excellent DPPH scavenging activities with the IC50 of 151.9 and 275.6 μg/mL, respectively, which were stronger than that of l-ascorbic acid (positive control) with the IC50 of 297.1 μg/mL. Additionally, these two most potent antioxidants were detectable in rat plasma after oral administration. In conclusion, this study reported important clues for the further pharmacological and clinical studies of YXST. Meanwhile, it provided a practical strategy for rapid screening and identifying of in vivo antioxidant in traditional Chinese medicine preparations.
Co-reporter:Keqiu Jiang, Peng Huang, Lianjun Luan, Kai Fan, Wenbo Guo, Zhihui Zhao, Yongjiang Wu, Zheng Han
Journal of Chromatography A 2017 Volume 1482(Volume 1482) pp:
Publication Date(Web):27 January 2017
DOI:10.1016/j.chroma.2016.12.058
•Fe3O4/MWCNT composite was synthesized and used as the SPE sorbent.•SPE was proposed for clean-up of mycotoxins in TCM Danshen.•UHPLC–MS/MS detection combined with SPE procedure provided a rapid determination.•Desirable levels of sensitivity, recovery and precision were achieved.For the first time, a reliable solid-phase extraction (SPE) procedure using iron (II, III) oxide (Fe3O4)/multi-walled carbon nanotube (MWCNT) composite as sorbents was proposed for purification and enrichment of zearalenone (ZEA) and four type A trichothecenes (T-2 toxin (T-2), HT-2 toxin (HT-2), neosolaniol (NEO) and diacetoxyscirpenol (DAS)) in Salviae miltiorrhiza Radix et Rhizoma (Danshen). The Fe3O4/MWCNT composite was synthesized by assembling Fe3O4 with MWCNT by sonication through an “aggregation wrap” mechanism and several key parameters affecting the performance of SPE procedure such as the composition of sample loading solutions, washing and elution solvents were thoroughly investigated. After optimization, 2% acetonitrile aqueous solution as the loading solution, 5% methanol aqueous solution as the washing solution and acetone containing 0.5% formic acid as the elution solvent presented an excellent purification efficiency for the five targets in Danshen. Under the optimal sample pretreatment conditions followed by analysis with ultra-high performance liquid chromatography-tandem mass spectrometry, satisfactory linearity (R2 ≥ 0.991), high sensitivity (limit of quantification in the range of 1.20–4.80 μg kg−1), good recovery (73.7–91.9%) and acceptable precision (RSD, 2.1–13.3%) were obtained. The applicability of the validated method was further verified in real Salviae miltiorrhiza Radix et Rhizoma samples.
Co-reporter:Yerui Li, Bowen Liu, Shu Geng, Sungchan Kim, Ye Jin, Xuesong Liu, Lianjun Luan, Yongjiang Wu, Yong Chen
Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 2016 Volume 157() pp:186-191
Publication Date(Web):15 March 2016
DOI:10.1016/j.saa.2016.01.001
•RTRT and NIR were combined to improve the quality control efficiency of TCM materials.•We established reliable NIR models for both quantitative and qualitative RTRT of Rhizoma paridis.•The quantitative RTRT outperformed qualitative RTRT with higher accuracy.Raw material examination is a critical process in the industrial production of traditional Chinese medicine (TCM); high accuracy and minimal time consumption are both required. In this study, near-infrared (NIR) spectroscopy was applied to improve the quality control efficiency of Rhizoma paridis. Partial least squares regression (PLSR) was first used to develop quantitative calibration models, and the discriminant analysis model was established to qualitatively discriminate the qualified samples from the unqualified samples. These two established NIR models were applied for real-time release testing (RTRT) of R. paridis. R. paridis saponins (RPS) ≥ 0.6% and moisture ≤ 12% were used as the quantitative releasing criteria of RTRT according to the Chinese Pharmacopoeia. Qualified samples classified by the discriminant analysis model were deemed to meet the qualitative releasing criterion of RTRT. Using the established quantitative model, 24 samples were allowed to be released to the subsequent production processes with 100% accuracy. For the qualitative RTRT analysis, three samples were misclassified as the unqualified class and were released unsuccessfully, the accuracy of the qualitative RTRT was 90%. Therefore, the quantitative RTRT was more feasible for actual manufacturing processes. Based on this study, a rapid and effective quantitative NIR spectroscopic method was proposed for the RTRT of R. paridis. The combination of RTRT and NIR spectroscopy could be a potential tool to improve the quality control efficiency of R. paridis.Graphical abstract
Co-reporter:Qiyuan Shi, Shu Geng, Jiale Chen, Qinfen Zhou, Ye Jin, Houliang Lei, Lianjun Luan, Xuesong Liu, Yongjiang Wu
Separation and Purification Technology 2015 Volume 153() pp:84-90
Publication Date(Web):16 October 2015
DOI:10.1016/j.seppur.2015.08.037
•An efficient method for the extraction of acylated pentasaccharides was proposed.•The extraction yields of acylated pentasaccharides were improved by more than 38.9%.•Three main acylated pentasaccharides were prepared by semi-preparative HPLC.In the present study, an efficient preparative procedure was developed for the preparation of three main acylated pentasaccharides from Polygalae Radix using integrated extraction–adsorption method followed by semi-preparative high performance liquid chromatography. Firstly, the acylated pentasaccharides were simultaneously extracted and purified by column chromatographic extraction integrated with macroporous resin purification. Comparing this integrated process to conventional one, some obvious advantages were observed, namely more than 38.9% enhancement of the recovery of acylated pentasaccharides, about 49.4% and 50.4% reduction in water and ethanol consumption, respectively. And then, the obtained extracts were further purified by semi-preparative high performance liquid chromatography. Finally, three known acylated pentasaccharides were purified from 100 g of Polygalae Radix, including tenuifoliose I (13 mg), tenuifoliose H (15 mg), and tenuifoliose A (21 mg). The purities of the compounds were determined by high performance liquid chromatography and the chemical structures were confirmed by mass spectrometric and NMR analysis.
Co-reporter:Yerui Li;Kai Yang;Qiyuan Shi;Bowen Liu;Ye Jin;Xuesong Liu;Zuolin Jiang;Lianjun Luan
Journal of Separation Science 2015 Volume 38( Issue 17) pp:2989-2994
Publication Date(Web):
DOI:10.1002/jssc.201500440
A simple and reliable method of high-performance liquid chromatography with diode array detection method was developed for fingerprint analysis and simultaneous determination of six compounds including puerarin, salvianolic acid B, berberine hydrochloride, palmatine chloride, dehydrocorydaline, and icariin in the Chinese medicine preparation Yangxinshi Pian. The separation was performed on an Agilent Eclipse XDB-C18 reserved-phase column (250 mm × 4.6mm I.D., 5 μm) using gradient elution with 50 mmol/L monopotassium phosphate aqueous solution and methanol as mobile phase at a flow rate of 1.0 mL/min. The column operating temperature was set at 30°C, and the detection wavelength was 280 nm. The method was validated by linearity, precision, accuracy, stability, and recovery. For fingerprint analysis, 25 peaks were selected as the common peaks, and four kinds of similarities including cosine similarity (S), ratio of similarity (S′), projection content similarity (C), and content similarity (P) were applied to evaluate the quality consistency of different batches of Yangxinshi Pian. The results showed that the developed method was an efficient tool for quality evaluation of Yangxinshi Pian.
Co-reporter:Xuesong Liu, Zengzeng Wu, Kai Yang, Haiying Ding, Yongjiang Wu
Journal of Pharmaceutical and Biomedical Analysis 2013 Volume 76() pp:70-74
Publication Date(Web):25 March 2013
DOI:10.1016/j.jpba.2012.12.013
A simple, reliable method for simultaneous determination of the ten components in Danhong injection (DHI) in combination of chromatographic fingerprint analysis was developed by high performance liquid chromatography coupled with diode-array-detector (HPLC-DAD). The separation was performed on an Agilent Zorbax SB-C18 column with a linear gradient elution of acetonitrile and 0.5% formic acid. The method was validated by linearity, precision, stability and recovery. The developed method was subsequently applied to evaluate 15 batches of DHI and testified to be suitable for its quality control.Graphical abstractThe figure is the fingerprint chromatograms of Danhong injection samples. In this research, four algorithms, namely cosine ratio, correlation coefficient, similarity ratio, and M value were applied for both qualitative and quantitative similarity evaluation, which would contribute to a more comprehensive assessment of the quality of DHI.Highlights► We established a method for both quantitative and qualitative analysis of Danhong injection. ► More comprehensive by using four algorithms in similarity evaluation of Danhong injection. ► Adopt a new parameter to reflect the consistency between batches to batches. ► Principal component analysis was applied to investigate the differentiation between samples.
Co-reporter:Ye Jin, Zengzeng Wu, Xuesong Liu, Yongjiang Wu
Journal of Pharmaceutical and Biomedical Analysis 2013 Volume 77() pp:32-39
Publication Date(Web):15 April 2013
DOI:10.1016/j.jpba.2013.01.012
The application of near infrared (NIR) spectroscopy for on-line quantitative monitoring of alcohol precipitation of the Danhong injection was investigated. For the NIR measurements, two fiber optic probes designed to transmit NIR radiation through a 2 mm path length flow cell were applied to collect spectra in real-time. Particle swarm optimization- (PSO-) based least square support vector machines (LS-SVM) and partial least squares (PLS) models were developed for quantitative analysis of the critical intermediate quality attributes: the soluble solid content (SSC) and concentrations of danshensu (DSS), protocatechuic aldehyde (PA), hydroxysafflor yellow A (HSYA) and salvianolic acid B (SAB). The optimal models were then used for on-line quantitative monitoring of alcohol precipitation. The results showed that the PSO-based LS-SVM with a radial basis function (RBF) kernel was slightly better than the conventional PLS method, even though both methods exhibited satisfactory fitting results and predictive abilities. In this study, successful models were built and applied on-line; these models proffer real-time data and instant feedback about alcohol precipitation.Graphical abstractHighlights► NIR spectroscopy was applied to on-line monitoring of alcohol precipitation. ► PSO was used to optimize the hyper-parameters of LS-SVM model. ► LS-SVM and PLS models were developed for five critical quality attributes. ► PSO based LS-SVM provided slightly better fitting results and prediction accuracy.
Co-reporter:Ye Jin, Haiying Ding, Xuesong Liu, Xinmin Wan, Lianjun Luan, Yongjiang Wu
Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 2013 Volume 109() pp:68-78
Publication Date(Web):15 May 2013
DOI:10.1016/j.saa.2013.02.014
An on-line detection method combining near infrared (NIR) spectroscopy with local partial least squares regression (PLSR) was investigated for the elution process of sodium aescinate. A 2 mm pathlength flow cell which transmitted NIR radiation through two fiber optic probes was placed in bypass of the macroporous resin column to collect real-time spectra of the sodium aescinate eluate. To compare the predictive accuracy, both local and global PLSR were employed to build mathematical models between NIR spectra and reference values. Meanwhile, Mahalanobis distance was introduced to select the appropriate local model for the prediction of unknown samples. Experimental results demonstrated that local PLSR was superior to global PLSR in both calibration performance and predictive accuracy. Moreover, the on-line detection method was proven to be feasible in real application and thereby would be of great value for monitoring the elution process of sodium aescinate in real time as well as determining the start and end points of eluate collection.Graphical abstractHighlights► We invested an on-line NIR method for elution process of sodium aescinate. ► Local PLSR models were developed and proved to be superior to the global model. ► Local PLSR models can be applied to on-line detection of elution process. ► Start and end points of elution process can be quickly determined by NIR. ► Model updating is efficient in dealing with deceased accuracy of original models.
Co-reporter:Yunliang Zheng, Lianjun Luan, Yong Chen, Yiping Ren, Yongjiang Wu
Journal of Pharmaceutical and Biomedical Analysis 2012 Volume 71() pp:54-62
Publication Date(Web):December 2012
DOI:10.1016/j.jpba.2012.08.020
Physalins are important bioactive compounds from genus Physalis. They often occur as isomers, which makes the structural elucidation difficult. In the present study, the fragmentation behavior and UV characteristics of seven physalins from genus Physalis were firstly investigated using electrospray ionization tandem mass spectrometry (ESI-MS/MS) and diode array detection (DAD). Combined with ultra-performance liquid chromatography (UPLC) and DAD, the established approach to the structural identification of physalins by ESI-MS/MS was then applied to the analysis of Physalis alkekengi L. According to the UPLC retention behavior, the diagnostic UV spectra and the molecular structural information provided by MS/MS spectra, about 19 fingerprint peaks were identified, including 14 physalins and 5 other compounds. Finally, the established fingerprint method was applied to the analysis of 31 P. alkekengi L. samples collected from different locations, which reflected their similar chemical constituent properties. The proposed method provides a scientific and technical platform to the herbal industry for quality control and safety assurance of herbal preparations that contain this class of physalins.
Co-reporter:Zheng Han, Yiping Ren, Junfeng Zhu, Zengxuan Cai, Yong Chen, Lianjun Luan, and Yongjiang Wu
Journal of Agricultural and Food Chemistry 2012 Volume 60(Issue 33) pp:8233-8247
Publication Date(Web):July 23, 2012
DOI:10.1021/jf301928r
A generic procedure, which involved accelerated solvent extraction and homemade cleanup cartridges, has been developed for the extraction and purification of 35 mycotoxins in various traditional Chinese medicine (TCM) matrixes, i.e., rhizomes and roots, seeds, flowers, and grasses and leaves, for subsequent analysis by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). All target analytes could be simultaneously quantitated in less than 17 min per run, showing narrow symmetrical peaks. The developed method was also successfully applied in routine monitoring programs, which implied a significant reduction of both effort and time, to investigate the contamination of TCMs. Among 60 commercial TCMs analyzed, 50 were positive. The achieved data underpin the practical application of the UHPLC–MS/MS method as a valuable tool for the trace analysis of multiple mycotoxins in TCMs.
Co-reporter:Yunliang Zheng;Yong Chen;Yiping Ren;Lianjun Luan
Phytochemical Analysis 2012 Volume 23( Issue 4) pp:337-344
Publication Date(Web):
DOI:10.1002/pca.1363
ABSTRACT
Introduction
Chinese lantern is the calyx or calyx-with-fruit of the plant Physalis alkekengi .var. franchetii (Solanaceae), and is potential material for the food and pharmaceutical industries. Physalins are the most active and representative secondary metabolites of Chinese lantern. A separation and quantification method based on UPLC-ESI-MS/MS was developed for the quantitative analysis of five active physalins. The transformation products were also detected and identified for the first time.
Objective
To establish a LC-MS/MS method to quantify five physalins in Chinese lantern for the purpose of quality control, and to identify the transformation products of 4,7-didehydrophysalin B.
Methodology
The separation was carried out on an Acquity UPLC BEH Shield RP C18-column with water and acetonitrile as the mobile phase under gradient conditions. ESI-MS/MS was used as the detector to quantify the five physalins. The transformation products of 4,7-didehydroneophysalin B were detected by UPLC–PDA-ESI-MS/MS and identified through comparing their HRMS and MS2 ion fragmentations with corresponding references.
Results
All the compounds showed good linearity (R2 > 0.998). The recoveries, measured at three concentration levels, varied from 98.8 to 101.4% with RSDs < 4.5%. The total contents of the five physalins in Chinese lantern varied significantly. Three transformation products of 4,7-didehydroneophysalin B were detected and tentatively identified.
Conclusion
The present study developed a highly effective analytical method for the quality control of Chinese lantern, and it could provide comprehensive information for quality evaluation and new drug development of Chinese lantern. Copyright © 2011 John Wiley & Sons, Ltd.
Co-reporter:Yunliang Zheng, Yong Chen, Yiping Ren, Lianjun Luan, Yongjiang Wu
Journal of Pharmaceutical and Biomedical Analysis 2012 58() pp: 94-101
Publication Date(Web):
DOI:10.1016/j.jpba.2011.09.012
Co-reporter:Zheng Han, Yiping Ren, Hailong Zhou, Lianjun Luan, Zengxuan Cai, Yongjiang Wu
Journal of Chromatography B 2011 Volume 879(5–6) pp:411-420
Publication Date(Web):15 February 2011
DOI:10.1016/j.jchromb.2010.12.028
A rapid and reliable ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method for simultaneous determination of zearalenone (ZEN), α-zearalenol (α-ZOL), β-zearalenol (β-ZOL), zearalanone (ZAN), α-zearalanol (α-ZAL) and β-zearalanol (β-ZAL) in traditional Chinese medicines (TCMs) was developed. The development of the method and investigations of the matrix influence were described in particular. After evaluation of the matrix effects of different TCMs, i.e., rhizomes and roots, seeds, flowers, grasses and leaves, by the post-extraction spiked method, a reliable sample clean-up method based on home-made clean-up cartridges, a suitable internal standard and the matrix calibration were combined using to minimize the matrix effects to ensure the accuracy of the method. The established method was further validated by determining the linearity (R2 ≥ 0.9990), sensitivity (limit of quantitation 0.11–0.99 ng mL−1), average recovery (86.6–113.5%) and precision (relative standard deviation ≤13.5%). It was shown to be a suitable method for simultaneous determination of ZEN, α-ZOL, β-ZOL, ZAN, α-ZAL and β-ZAL in different TCMs. Finally, the established method was successfully applied to the determination of the six mycotoxins in various TCMs and the results were presented to provide relevant insights to researchers in TCM analysis.
Co-reporter:Yiping Ren, Zheng Han, Xiaojun Chu, Jingshun Zhang, Zengxuan Cai, Yongjiang Wu
Analytica Chimica Acta 2010 Volume 667(1–2) pp:96-102
Publication Date(Web):14 May 2010
DOI:10.1016/j.aca.2010.04.015
A reliable ultra-high-performance liquid chromatography–mass spectrometry method for simultaneous determination of bovine α-lactalbumin (α-La) and β-lactoglobulin (β-Lg) was developed. Compared to the previous methods, the developed approach with mass spectrometer operated in selected area monitoring mode offered increased speed and enhanced lower detection limit. A linear gradient mobile phase, consisting of (A) water containing 0.1% trifluoroacetic acid (TFA) and (B) acetonitrile containing 0.1% TFA, and an Acquity UPLC BEH300 C18 column (150 mm × 2.1 mm, 1.7 μm) were employed to obtain the best resolution of the target analytes. The accurate quantitation was achieved by employing human α-lactalbumin as the internal standard. The established method was extensively validated by determining the linearity (R2 ≥ 0.9991), sensitivity (limit of quantitation, 0.15–0.19 μg mL−1), recovery (94.0–98.7%), precision (relative standard deviation ≤ 11.1%) and repeatability (relative standard deviation ≤ 5.7%). It was shown to be a suitable method for simultaneous determination of the major whey proteins in biological samples. Current validated method was successfully applied to the nutrient investigation of infant formulae.
Co-reporter:Zheng Han, Yunliang Zheng, Lianjun Luan, Zengxuan Cai, Yiping Ren, Yongjiang Wu
Analytica Chimica Acta 2010 Volume 664(Issue 2) pp:165-171
Publication Date(Web):7 April 2010
DOI:10.1016/j.aca.2010.02.009
An ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) method for simultaneous determination of aflatoxins B1, B2, G1, G2, M1 and M2 in traditional Chinese medicines (TCMs) was developed. The approach was characterized in details and a special focus was placed on the recovery rates of isolation procedure in different TCM matrices, i.e. rhizomes and roots, seeds, flowers, grasses and leaves. For this purpose, [13C17]-aflatoxinB1 was employed as the internal standard and a reliable solid phase extraction-based clean-up method was developed. The observed recovery rates of the six aflatoxins ranged from 85.6% to 117.6% in different matrices. Then, the established method was successfully applied to the determination of the six aflatoxins in various TCMs. For 30 commercial samples analyzed, 16 were contaminated with aflatoxins. The mean levels (incidence) of aflatoxins B1, B2, G1 and G2 in positive samples were 1.40 (68.8%), 1.27 (50.0%), 0.50 (43.8%) and 0.94 (43.8%) μg kg−1, respectively. Interestingly, aflatoxin M1 was detected in two samples with the maximal content of 0.70 μg kg−1. No sample was contaminated with aflatoxin M2. Meanwhile, a possible association between the contamination levels and the selected herbs was clarified in the present study.
Co-reporter:Zheng Han, Yunliang Zheng, Lianjun Luan, Yiping Ren, Yongjiang Wu
Journal of Chromatography A 2010 Volume 1217(Issue 26) pp:4365-4374
Publication Date(Web):25 June 2010
DOI:10.1016/j.chroma.2010.04.052
The paper reported a reliable analytical method for simultaneous determination of ochratoxin A (OTA) and ochratoxin B (OTB) in traditional Chinese medicines (TCMs) by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). The development of the method and investigations on the matrix influence were described in particular. The matrix effects were thereby minimized by using a reliable internal standard and a simple sample pretreatment. The established method was further validated by determining the linearity (R2 ≥ 0.9990), average recovery (86.3–114.2%), sensitivity (limit of quantitation 0.03–0.19 ng mL−1) and precision (relative standard deviation ≤ 13.1%). It was shown to be a suitable method for simultaneous determination of OTA and OTB in various TCMs. Finally, a total of 51 TCMs widely used in China were screened for OTA and OTB with the proposed method. The results showed that only 4 samples were contaminated with ochratoxins at low levels, indicating that it was low risk of ochratoxins to consumers who occasionally used TCMs.
Co-reporter:Zheng Han;Xuesong Liu;Yiping Ren;Lianjun Luan
Journal of Separation Science 2010 Volume 33( Issue 13) pp:1923-1932
Publication Date(Web):
DOI:10.1002/jssc.201000094
Abstract
A speedy and selective ultra-HPLC-MS/MS method for simultaneous determination of deoxynivalenol (DON), 3-acetyldeoxynivalenol (3-ADON), 15-ADON, nivalenol and fusarenon X in traditional Chinese medicines (TCMs) was developed. The method was based on one-step sample cleanup using reliable homemade cleanup cartridges. A linear gradient mobile-phase system, consisting of water containing 0.2% aqueous ammonia and acetonitrile/methanol (90:10, v/v) at a flow rate of 0.4 mL/min, and an Acquity UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) were employed to obtain the best resolution of the target analytes. [13C15]–DON was used as the internal standard to accomplish as accurate as possible quantitation. The established method was further validated by determining the linearity (R2≥0.9990), sensitivity (LOQ, 0.29–0.99 μg/kg), recovery (88.5–119.5%) and precision (RSD≤15.8%). It was shown to be a suitable method for simultaneous determination of DON, 3-ADON, 15-ADON, nivalenol and fusarenon X in various TCM matrices. The utility and practical impact of the method was demonstrated using different TCM samples.
Co-reporter:Zheng Han;Yiping Ren;Xuesong Liu;Lianjun Luan
Journal of Separation Science 2010 Volume 33( Issue 17-18) pp:2723-2733
Publication Date(Web):
DOI:10.1002/jssc.201000423
Abstract
A reliable isotope dilution method for simultaneous determination of fumonisin B1, fumonisin B2 and fumonisin B3 in traditional Chinese medicines by ultra-high-performance LC-MS/MS was developed, and a special focus was placed on the optimization of extraction, cleanup, ultra-high-performance LC separation and MS/MS conditions. Homogenized samples were extracted by 50% acetonitrile aqueous solution and purified with MultiSep 211 Fum columns. A linear gradient mobile phase, consisting of water containing 0.2% formic acid and acetonitrile/methanol (50:50 v/v) and an Acquity UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) were employed to obtain the best resolution of the analytes for the positive ESI+ analysis. The established method was validated by determining the linearity (R2≥0.9991), sensitivity (LOQ, 0.08–0.16 ng/mL), recovery (88.2–113.3%) and precision (RSD≤12.3%). Finally, the validated method was successfully applied to the determination of fumonisins in different traditional Chinese medicines. Of 35 samples, 18 were contaminated with fumonisins. The mean levels (incidence) of fumonisin B1, fumonisin B1 and fumonisin B1 in positive samples were 8.55 (94.4%), 4.88 (77.8%) and 0.52 μg/kg (33.3%), respectively. Based on the contaminant situations, a possible association between the contamination levels and the selected herbs was clarified in this study.
Co-reporter:Yunliang Zheng, Xuesong Liu, Lianjun Luan, Longhu Wang, and Yongjiang Wu
Journal of Chemical & Engineering Data 2010 Volume 55(Issue 9) pp:3690-3692
Publication Date(Web):April 26, 2010
DOI:10.1021/je100227k
The solubility of physalin D in ethanol, methanol, propanone, trichloromethane, ethyl ethanoate, and water at temperatures from (283.2 to 313.2) K was measured under at a pressure of 0.1 MPa. The solubility of physalin D in these solvents increases with increasing temperature. The experimental solubility data were correlated with the Apelblat equation.
Co-reporter:Lian-Jun Luan;Fa-Ping Gan;Yong-Jiang Wu
Chromatographia 2008 Volume 68( Issue 9-10) pp:
Publication Date(Web):2008 November
DOI:10.1365/s10337-008-0763-7
A liquid chromatographic method for the simultaneous determination of three flavonoids, scutellarin (SCU), isoscutellarein-8-O-glucuronide (ISO) and luteolin (LUT) in rat plasma was developed and validated. Following a single-step liquid–liquid extraction with ethyl acetate, the analytes and internal standard (IS) (rutin) were successfully separated on a Diamonsil C18 column using a mobile phase composed of acetonitrile (A)–0.2% phosphoric acid aqueous solution (B) (0–5 min, 20% A–29% A; 5–25 min, 29% A, v/v) at a flow rate of 1.0 mL min−1. The linear range was 0.044–2.20 μg mL−1 for SCU, 0.042–2.08 μg mL−1 for ISO, and 0.056–2.80 μg mL−1 for LUT, with the correlation coefficients of 0.9995, 0.9989 and 0.9963, respectively. The limit of quantification of SCU, ISO and LUT were 44, 41.6 and 56 ng mL−1, respectively. The accuracy of assay was between 88.4 and 103.0%. The inter-day and intra-day precisions (RSD) were less than 10.5%. The developed method was simple, rapid and applied successfully to study the pharmacokinetics of SCU, ISO and LUT after oral administration of the total flavonoids of Scutellaria barbata.
Co-reporter:Zheng Han, Keqiu Jiang, Zhichen Fan, José Diana Di Mavungu, Maofeng Dong, Wenbo Guo, Kai Fan, Katrina Campbell, Zhihui Zhao, Yongjiang Wu
Food Control (September 2017) Volume 79() pp:177-184
Publication Date(Web):1 September 2017
DOI:10.1016/j.foodcont.2017.03.044
•Synthesis of MWCNT-MNPs and approaches for their use in M-SPE.•M-SPE was proposed for clean-up of zearalenone and its derivatives in maize.•UHPLC-MS/MS detection combined with M-SPE purification for rapid analysis.•Matrix effects were eliminated and matrix-matched calibration was unnecessary.•The approach provides the desirable level of sensitivity, recovery and precision.A simple and rapid magnetic solid-phase extraction (M-SPE) procedure using multi-walled carbon nanotube-magnetic nanoparticles (MWCNT-MNPs) as sorbents was established for purification of zearalenone (ZEA), α-zearalenol (α-ZOL), β-zearalenol (β-ZOL), zearalanone (ZAN), α-zearalanol (α-ZAL) and β-zearalanol (β-ZAL) in maize. The main parameters affecting the clean-up efficiency were thoroughly investigated, and high purification efficiencies for all analytes were obtained. The resulting MWCNT-MNP-ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was validated for maize samples. The matrix effects were greatly minimized using the M-SPE approach, with signal suppression/enhancement values decreased from 69.9–127.6% to 92.1–103.8%. Consequently, complex matrix-matched calibration curves were not necessary and the calibrations constructed in acetonitrile could be applied for accurate quantification of the targeted mycotoxins in real samples. The average recoveries ranged from 75.8 to 104.1% and the inter- and intra-day precision values expressed as RSDs, were all lower than 14%. Limits of detection and quantification were in the range of 0.03–0.04 and 0.07–0.10 μg/kg, respectively. The analytical performance of the developed method was also successfully evaluated with maize samples, and this method was proved to be a powerful tool for monitoring ZEA and its derivatives in maize.
![Benzenepropanoic acid, a-[[(2E)-3-[2-(carboxymethyl)-3,4-dihydroxyphenyl]-1-oxo-2-propen-1-yl]oxy]-3,4-dihydroxy-,(aR)-](http://img.cochemist.com/ccimg/143000/142998-47-8.png)
![Benzenepropanoic acid, a-[[(2E)-3-[2-(carboxymethyl)-3,4-dihydroxyphenyl]-1-oxo-2-propen-1-yl]oxy]-3,4-dihydroxy-,(aR)-](http://img.cochemist.com/ccimg/143000/142998-47-8_b.png)
![[(2R,3S,4S,5R,6R)-3,4,5-TRIHYDROXY-6-[(2R,3S,4R,5R)-4-HYDROXY-3-[(E)-3-(4-HYDROXY-3,5-DIMETHOXYPHENYL)PROP-2-ENOYL]OXY-2,5-BIS(HYDROXYMETHYL)OXOLAN-2-YL]OXYOXAN-2-YL]METHYL (E)-3-(4-HYDROXY-3,5-DIMETHOXYPHENYL)PROP-2-ENOATE](http://img.cochemist.com/ccimg/139900/139891-98-8.png)
![[(2R,3S,4S,5R,6R)-3,4,5-TRIHYDROXY-6-[(2R,3S,4R,5R)-4-HYDROXY-3-[(E)-3-(4-HYDROXY-3,5-DIMETHOXYPHENYL)PROP-2-ENOYL]OXY-2,5-BIS(HYDROXYMETHYL)OXOLAN-2-YL]OXYOXAN-2-YL]METHYL (E)-3-(4-HYDROXY-3,5-DIMETHOXYPHENYL)PROP-2-ENOATE](http://img.cochemist.com/ccimg/139900/139891-98-8_b.png)
![(2s,3s)-4-[(e)-3-[(1r)-1-carboxy-2-(3,4-dihydroxyphenyl)ethoxy]-3-oxoprop-1-enyl]-2-(3,4-dihydroxyphenyl)-7-hydroxy-2,3-dihydro-1-benzofuran-3-carboxylic Acid](http://img.cochemist.com/ccimg/28900/28831-65-4.png)
![(2s,3s)-4-[(e)-3-[(1r)-1-carboxy-2-(3,4-dihydroxyphenyl)ethoxy]-3-oxoprop-1-enyl]-2-(3,4-dihydroxyphenyl)-7-hydroxy-2,3-dihydro-1-benzofuran-3-carboxylic Acid](http://img.cochemist.com/ccimg/28900/28831-65-4_b.png)
![(1s,3r,4r,5r)-3,4-bis[[(e)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy]-1,5-dihydroxycyclohexane-1-carboxylic Acid](http://img.cochemist.com/ccimg/14600/14534-61-3.png)
![(1s,3r,4r,5r)-3,4-bis[[(e)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy]-1,5-dihydroxycyclohexane-1-carboxylic Acid](http://img.cochemist.com/ccimg/14600/14534-61-3_b.png)
![5-hydroxy-2-(4-methoxyphenyl)-7-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-[[(2r,3r,4r,5r,6s)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxymethyl]oxan-2-yl]oxychromen-4-one](http://img.cochemist.com/ccimg/500/480-36-4.png)
![5-hydroxy-2-(4-methoxyphenyl)-7-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-[[(2r,3r,4r,5r,6s)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxymethyl]oxan-2-yl]oxychromen-4-one](http://img.cochemist.com/ccimg/500/480-36-4_b.png)
![a-D-Glucopyranoside,3-O-[(2E)-3-(4-hydroxy-3,5-dimethoxyphenyl)-1-oxo-2-propen-1-yl]-b-D-fructofuranosyl,6-(4-hydroxybenzoate)](http://img.cochemist.com/ccimg/139800/139726-36-6.png)
![a-D-Glucopyranoside,3-O-[(2E)-3-(4-hydroxy-3,5-dimethoxyphenyl)-1-oxo-2-propen-1-yl]-b-D-fructofuranosyl,6-(4-hydroxybenzoate)](http://img.cochemist.com/ccimg/139800/139726-36-6_b.png)
