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Zhang R.,China Pharmaceutical University | Zhang R.,Jiangxi University of Traditional Chinese Medicine | Wang Y.,China Pharmaceutical University | Wang Y.,Jiangsu Institute for Food and Drug Control | And 3 more authors.
Journal of Chromatographic Science | Year: 2012

The chemical composition of polysorbate 80 strongly influences the physicochemical properties and performance of many products. Consequently, a reliable characterization of polysorbate 80 is crucial for many applications. However, the exact composition of these chemical mixtures cannot be determined by colorimetry, hydrolysis, size-exclusion chromatography, nuclear magnetic resonance or mass spectrometry (MS). Meanwhile, due to the strong retention of higher esters on the reversed-phase (RP) column, the published high-performance liquid chromatography (HPLC) methods suffered from inadequate elution. In the present paper, an HPLC-evaporative light scattering detection (ELSD) and an HPLC-electrospray ionization (ESI)-MS method were developed and validated for the separation and identification of the chemical composition of polysorbate 80. A full separation of the entire composition was achieved in 45 min. In the HPLC-ESI-MS spectra, each class of the compound in polysorbate 80 was directly confirmed and identified by [M 1 NH4]1 and [M 1 2NH4]-1 ions. The number of polyoxyethylene groups and their distribution within the molecule were determined, in addition to the dehydration and esterification degree of sorbitol. Analysis showed that polysorbate 80 contained different proportions of components (polyoxyethylene sorbitan, polyoxyethylene isosorbide, polyoxyethylene sorbitan monooleate-dioesters-trioleates-tetraoleates and polyoxyethylene isosorbide monoester-dioesters). It was concluded that HPLC-ESI-MS is a useful tool for establishing the compositional profile of polysorbate 80. © The Author [2012]. Published by Oxford University Press. All rights reserved.

Zou L.,China Pharmaceutical University | Li X.,China Pharmaceutical University | Shi Q.,Jiangsu Institute for Food and Drug Control | Feng F.,China Pharmaceutical University
Analytical Methods | Year: 2014

Zhi-Zi-Da-Huang decoction (ZZDHD) is an effective formula to treat alcoholic liver disease in China for nearly 2000 years. However, compounds in the formula are still not clear due to the complexity of the coexisting constituents. In this study, a sensitive integrated method based on HPLC-DAD-ESI-MS (TOF) and HPLC-DAD-ESI-MS/MS (QqQ) was developed and 85 chemical compounds in ZZDHD were identified. By TOF/MS, the quasi-molecular ions of the constituents were deduced according to the accurate mass of corresponding positive and negative ions, and product ion scan was then carried out using QqQ/MS. The fragments of each compound were observed by TOF/MS and/or QqQ/MS. Compounds with different chemical structures and concentration levels were tentatively identified according to their chromatographic retention time, UV absorption and MS data. Fragmentation patterns of six types were proposed to verify the identification results. It was found that at TOF/MS mode, a retro diels-alder (RDA) reaction occurred at bonds 1 and 3 in C-ring of flavanone 7-O-diglycosides when 4′-OH exists at B-ring. While the reaction was not observed if a methoxyl group appeared at the same site of flavanone skeleton. Another important phenomenon was noticed that 3-sinapoyl-5-caffeoylquinic acid, 4-sinapoyl-3-caffeoylquinic acid, and sinapylglucoside were detected only in ZZDHD while they were not found in four component herb extracts. The phenomenon revealed that changes of compounds happened when the component herbs were decocted together. The results in the paper are favorable of the clinic dosage and have laid a foundation for the subsequent research of ZZDHD in vivo. © 2014 the Partner Organisations.

An L.,China Pharmaceutical University | Shi Q.,Jiangsu Institute for Food and Drug Control | Feng F.,China Pharmaceutical University
RSC Advances | Year: 2015

Zhi-Zi-Da-Huang decoction (ZZDHD), a Traditional Chinese Medicine (TCM) formula, has been widely used for the treatment of alcohol-induced liver injury for many years. To comprehensively explore the possible mechanism of the hepatoprotective effects of ZZDHD, a nuclear magnetic resonance (NMR)-based metabolomics study, 1H NMR spectra combined with pattern recognition methods including PCA and OPLS-DA, was applied to identify potential plasma and liver biomarkers responsible for the positive effects of ZZDHD on alcohol-induced liver injury in rats. PCA gave a global overview of control, alcohol and ZZDHD group rats. Potential plasma and liver biomarkers that were obtained from OPLS-DA loading plots combined with the corresponding VIP values reflected the hepatoprotective effects of ZZDHD associated with alcohol-induced liver injury. The results suggested that 9 potential plasma biomarkers including, lipoprotein, leucine, valine, dihydrothymine, 3-d-hydroxybutyrate, lactate, alanine, acetate and glucose, and 8 potential liver biomarkers, triglyceride, lactate, alanine, acetate, glutamine, glucose, xanthine and hypoxanthine were identified. Related metabolic pathway analysis found that ZZDHD significantly alleviated the disturbance in energy metabolism, glucose metabolism, amino acid metabolism, lipid metabolism, nucleic acid metabolism, ameliorating lipid peroxidation and permeability change of membrane, and oxidative stress induced by alcohol. The results indicated that ZZDHD could achieve remarkable effects on alcoholic hepatic injury through partially preventing or regulating the perturbed metabolic pathways. The study also demonstrated that NMR-based metabolomics was a useful tool for screening potential biomarkers, further helping to explain the therapeutic mechanism of TCM formula on a comprehensive scale. © 2015 Royal Society of Chemistry.

Lu L.,Jiangsu Institute for Food and Drug Control | Gong X.,Jiangsu Institute for Food and Drug Control | Feng Y.,Jiangsu Institute for Food and Drug Control
Chinese Journal of Chromatography (Se Pu) | Year: 2014

A method for the analysis of sixteen phthalate acid ester (PAE) residues in health wine was developed using gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS). The health wine samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The samples were detected by GC-QQQ-MS with electron impact source (EI) in selected ion monitoring (SIM) mode after extraction. The separation was performed on an HP-5MS capillary column (30 m ×0. 25 mm ×0. 25 μm) with temperature programming. The retention time and the fragment ion abundance ratio were used to judge the qualitative results, and the quantitation was performed with standard curve method of the characteristic ion chrom-atographic peak area-concentration. Eighty-one batches of health wine samples were detected using the method. The results showed that the method had good linear relationships with corre-lation coefficients (r2) not less than 0. 995 9. The recoveries of fifteen PAEs ranged from 88. 6% to 107. 3% except dimethyl phthalate (DMP) which was 52. 3% -58. 7% in all the three spiked levels with the relative standard deviations of 0. 1% -6. 8% (RSD, n =6). The limits of detection were between 0. 002 mg/L to 0. 061 mg/L. The limits of quantification were between 0. 005 mg/L and 0. 202 mg/L. The method is accurate, sensitive, proprietary and suitable for the simultaneous determination of the sixteen phthalate acid esters in health wine.

Zhang L.,Jiangsu Institute for Food and Drug Control | Zhang L.,Nanjing University | Shang C.,Nanjing University | Sun C.,Nanjing University
Chinese Journal of Chromatography (Se Pu) | Year: 2014

Phthalate esters (PAEs) are commonly used for plastic products as plasticizer. Once taken in by human, PAEs will cause diseases, such as endocrine disorders, cancer, etc. Shengmaiyin is a kind of Chinese medicine oral fluid whose packaging materials may include phthalate esters. If the phthalate esters migrated into the solution, it would lead to serious problem on the safety of drugs. In this study, a method of gas chromatography coupled to triple quadrupole mass spectrometry (GC-QQQ-MS) was developed for the simultaneous determination of 17 phthalate esters in Shengmaiyin samples. The samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The separation was performed on an HP-5MS capillary column (30 m×0. 25 mm×O. 25 μm) with temperature programming. The MS/MS detection was performed under electron impact source (EI) in multi-reaction monitoring (MRM) mode. The good linear relationships were obtained in the range of 0. 5-20 mg/L for all the target analytes. The average recoveries of the 15 PAEs were in the range of 91. 8% -117. 2%, except dimethyl phthalate and diethyl phthalate which were about 51. 9% and 77. 2%, respectively, and all the RSDs were in the range of 0. 5%-5. 4% (n = 6). The limits of detection ranged from 0. 04 to 16. 76 μg/L. The developed GC-MS method is simple, accurate, sensitive, proprietary, and can be applied in the detection of the phthalate ester residues in Shengmaiyin.

Deng X.,Catholic University of Leuven | Yuan Y.,Jiangsu Institute for Food and Drug Control | Adams E.,Catholic University of Leuven | Van Schepdael A.,Catholic University of Leuven
Talanta | Year: 2013

A fast and sensitive chiral capillary electrophoresis method has been developed to determine levornidazole and its enantiomeric impurity at a 0.05% level in levornidazole injection solution. Several chemical and instrumental parameters which have an effect on chiral separation were investigated, including chiral selectors, buffer composition and pH, applied voltage, capillary length, temperature and rinsing procedure. After optimizing all the effective parameters, the ideal separation conditions were 20 mM Tris phosphate buffer at pH 2.1, containing 2.0% (w/v) sulfated-α-cyclodextrin with short end injection at 0.5 psi for 5.0 s. Online UV detection was performed at 277 nm. A voltage of 30 kV was applied and the capillary temperature was kept at 25 °C. 2,4,6-triaminopyrimidine was chosen as internal standard to improve the injection precision. The total analysis time is less than 7 min, which is faster than the existing chiral HPLC method (65 min). The validation of the method was performed in terms of factorial analysis, stability of the solution, different cyclodextrin batches study, selectivity, linearity (from 2.5 μg/mL to 6000 μg/mL, y=0.0015 x+0.0304; R2=0.9999 and the residuals were randomly scattered around 0), LOD and LOQ (0.3 and 1.0 μg/mL, respectively), precision and accuracy. The proposed method was then applied to the enantiomeric purity control of the starting material and injection solution of levornidazole (0.5 mg/100 mL). © 2012 Elsevier B.V.

Yang F.,China Pharmaceutical University | Du Y.,China Pharmaceutical University | Chen B.,China Pharmaceutical University | Fan Q.,Jiangsu Institute for Food and Drug Control | Xu G.,China Pharmaceutical University
Chromatographia | Year: 2010

In this study, a new approach to the enantioseparation of nefopam hydrochloride by means of affinity electrokinetic chromatography (AEKC) with chondroitin sulfate A belonging to linear ionic polysaccharides has been developed. The difference in the antinociceptive activity of the enantiomers of nefopam was demonstrated in some studies, and the method established in this paper allowed complete separation of nefopam. Especially, there are no reports concerned with the enantioselective separation of nefopam using chondroitin sulfate A as chiral selectors in CE. During the course of this work, both migration time and enantioseparation of nefopam were influenced by several parameters such as pH of the BGE, selector concentration, capillary temperature and applied voltage. Consequently, these parameters were systematically optimized in order to obtain the optimum enantioseparation of nefopam. Moreover, comparison of the influences of the studied parameters was further investigated using univariate analysis of variance as a calculation method by Statistical Product and Service Solutions (SPSS) in this paper. Finally, a mechanism of enantiorecognition in AEKC towards the enantiomers of nefopam with chondroitin sulfate A was described. © 2010 Vieweg+Teubner Verlag | Springer Fachmedien Wiesbaden GmbH.

PubMed | Jiangsu Institute for Food and Drug Control and China Pharmaceutical University
Type: | Journal: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences | Year: 2016

Identification of metabolic profile of traditional Chinese medicine in vivo is always a challenge task. Usually, screening out and identifying the exogenous compounds manually from total ion chromatograms (TICs) of biologic samples is time-consuming and strenuous. In this study, a systematic identification strategy based on LC-MS was adopted to clarify the metabolic profiling of Zhi-Zi-Hou-Po decoction (ZZHPD) in rat. Bile, urine and feces samples of rat were obtained after oral administration and then analyzed by LC-MS after proper preparation. The xenobiotics were screened out from TICs globally and rapidly by untargeted metabolomics-driven strategy (UMDS) based on the combined of XCMS online (a web-based platform to process LC-MS data), MetAlign (a software to process LC-MS data) and SIMCA-P (a software for data analysis). Most of the xenobiotics were identified by means of series product ions filtering (sPIF), which was based on the database-hit of ZZHPD (including prototype and metabolites). Then the unmatched constituents were identified tentatively and their source and metabolic pathway were clarified by using diagnostic fragment ions strategy (DFIS). As a result, a total of 83 compounds including 44 prototype compounds and 39 metabolites were rapidly identified or tentatively characterized from the biologic samples, and among them, four of which were found for the first time. Further research on the correlations of these prototype compounds and metabolites revealed that glucuronidation is the main metabolic pathways of ZZHPD in rat bile and urine, while prototype compounds were the abundant ingredients detected in rat feces.

PubMed | Jiangsu Institute for Food and Drug Control and China Pharmaceutical University
Type: Journal Article | Journal: Journal of separation science | Year: 2016

Lonicerae Japonicae Flos is often adulterated with Lonicerae Flos, which is derived from the other four Lonicera species, in both the crude drug and Lonicerae Japonicae Flos preparations. We proposed a methodology for the quantitative analysis of adulterant Lonicerae Flos in Lonicerae Japonicae Flos preparations. Taking macranthoidins A, B, dipsacoside B (saponins), sweroside (iridoids), and luteolin-7-O-d-glucoside (flavonoids) as markers, a method of ultra high performance liquid chromatography with triple quadrupole mass spectrometry was employed to determine their amounts in Lonicerae Flos, Lonicerae Japonicae Flos, and Lonicerae Japonicae Flos preparations. The proportion of adulterant Lonicerae Flos in Lonicerae Japonicae Flos preparations was estimated based on the saponin contents of Lonicerae Japonicae Flos and Lonicerae Flos. All analytes separated under isocratic elution in 12 min with acceptable linearity, precision, repeatability, and accuracy. Lonicerae Japonicae Flos was easily distinguished from Lonicerae Flos by the total amount of saponins (0.067 and > 45.8 mg/g for Lonicerae Japonicae Flos and Lonicerae Flos, respectively). Eighteen of twenty one Lonicerae Japonicae Flos preparation samples were adulterated with Lonicerae Flos in proportions of 11.3-100%. The developed ultra high performance liquid chromatography with triple quadrupole mass spectrometry method could be used for the identification of Lonicerae Japonicae Flos and the four species of Lonicerae Flos and for the analysis of Lonicerae Japonicae Flos preparations adulterated with Lonicerae Flos.

PubMed | Jiangsu Institute for Food and Drug Control and China Pharmaceutical University
Type: | Journal: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences | Year: 2016

Zhi-Zi-Da-Huang decoction (ZZDHD) has been used for treatment of alcoholic liver disease in China for thousands of years. In order to reveal the dynamic biotransformation of the decoction in vivo, a high-throughout, sensitive and special method based on high performance liquid chromatography coupled with diode array detection and time-of-flight mass spectrometry (HPLC-DAD-TOF/MS) and high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QqQ/MS) was developed and validated. 25 parent compounds and 28 metabolites were characterized, among which, two metabolites were found for the first time and tentatively identified by neutral-loss scan and product-ion scan. All the compounds were assigned to iridoids, flavones, anthraquinones, coumarin or p-coumaric acid, and their biotransformation pathways were found to involve glucuronidation, sulfation, reduction and ring cleavage. Glucuronidation occurred as a major metabolic pathway of genipin and flavanone and the conjugates could be detected almost during the whole sampling duration. To compounds such as anthraquinones, coumarin and p-coumaric acid, sulfation is the only transformation pathway and the metabolites were found at 0-12, 4-18, 4-48h respectively after administration. Reduction and/or ring cleavage of genipin glucuronide and naringin were also observed obviously. The phenomena that parts of parent compounds and metabolites were able to be detected even 48h after administration implied that the accumulating effect of these constituents in vivo would happen and the potential toxicity of the decoction might appear if multiple dosing is adopted. The strategy used in this paper was proved helpful to offer important information for the clinical safe use of ZZDHD.

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