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HPLC/MS
FOOD CONTROL · 2022 · IF 6.652

Source identification of vanillin in sesame oil by HPLC-MS/MS

Mengying Wang,Yuepeng Lu,Yong Yang,Jiahao Yu,Yechao Chen,Fengqin Tu,Jing Hou,Zong Yang,Xiaoming Jiang

Recently, we found that vanillin commonly exists in sesame oils, while vanillin compounds are not allowed to be used as food additives in edible vegetable oils according to Chinese standards for Food Additives (GB2760-2014). To trace the source of vanillin in sesame oil, an accurate and reliable method was developed and validated for the determination of vanillin, methyl vanillin and ethyl vanillin in sesame samples based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The limit of determination (LOD) and limit of quantification (LOQ) of the established method were in the range of 17.4–33.1 and 52.2–99.2 μg kg −1 , respectively. The calibration curves of the three vanillin compounds exhibited good linearity between 0 and 400 ng mL −1 , with a high correlation coefficient greater than 0.999. The recoveries ranged from 91.7% to 112%, with a low relative standard deviation (RSD) less than 5.55%. Then this method was applied for the detection of sesame seed and intermediate samples. The results showed that all samples contained vanillin in a concentration range of 382–3804 μg kg −1 , while methyl vanillin and ethyl vanillin were not detected in those samples. Hence, the vanillin in sesame oil may originate from its raw materials, indicating that vanillin was not a good detection marker for illegal addition of flavor enhancers in sesame oils.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 食品安全 · 食品科学
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2022 · IF 4.52

Simultaneous determination of 20 phenolic compounds in propolis by HPLC-UV and HPLC-MS/MS

Yan Zhang,Cuiling Cao,Zhiwei Yang,Guangqun Jia,Xiaomao Liu,Xuemin Li,Zongyan Cui,Adan Li

Propolis is rich in flavonoids and phenolic acids , which has strong antioxidant capacity . Two methodologies for simultaneous determination of 20 phenolic compounds in propolis by HPLC-UV and HPLC-MS/MS were developed. The sample extraction and chromatographic separation conditions, and ultraviolet detection wavelength, as well as mass spectrometry parameters were selected and optimized. Under the optimized conditions, good linearities ( R 2 ≥0.998) were obtained for all analytes. The limits of quantification (LOQs) of the proposed methods by HPLC-UV and HPLC-MS/MS for all analytes were in the range of 0.02–0.1 mg/g and 0.05–0.2 mg/g, respectively, and the recoveries were in the range of 95.4 %− 109.5 % and 94.0 %− 106.8 % with the relative standard deviations (RSDs) in the range of 1.1 %− 7.5 % and 0.4 %− 11.1 %, respectively. The proposed methods were applied for the determination of 20 phenolic compounds in 13 propolis samples collected from China and Brazil. The detection results of the two methods are almost consistent with each other, indicating that both methods are applicable, and the inter-confirmation of the two methods can improve the accuracy of the determination of phenolic components in propolis.

研究领域: 植物化学 · 分析化学 · 药学
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2023 · IF 4.3

HPLC-MS/MS method for the simultaneous determination of lysine-derived markers for protein carbonylation in meat

Shouyin Wang,Shengjie Li,Wenhui Wang,Xiuxia Guo,Jinfeng Pan,Xiuping Dong

This paper aimed to develop a quantitative method based on high-performance liquid chromatography (HPLC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) for the simultaneous determination of two protein carbonylation products derived from lysine residues in meat proteins, namely, α-aminoadipic semialdehyde (AAS) and lysinonorleucine (LNL). Mass spectrometry conditions and derivatization parameters were optimized and the linearity, repeatability, bias, the limit of detection (LOD), the lower limit of quantification (LLOQ), and recovery were validated. The developed method showed satisfactory linearity, repeatability, and sensitivity for both AAS and LNL. This method was applied to analyze the contents of these compounds in different meat products, and the formation of AAS was observed to be closely related to the severity of the manufacturing conditions. Moreover, AAS was demonstrated to be a reliable but more sensitive marker for protein carbonylation compared to the DNPH method, which could also provide information regarding the specific pathway of protein carbonylation.

研究领域: 食品科学 · 分析化学
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Journal of Cotton Research · 2024 ·Vol. 7 ·期 1 ·1-14 · IF 3.1

Simultaneous determination of five plant hormones in cotton leaves using QuEChERS combined with HPLC‒MS/MS

Wang Wenhao,Song Xianpeng,Wang Dan,Ma Yajie,Shan Yongpan,Ren Xiangliang,Hu Hongyan,Wu Changcai,Yang Jun,Ma Yan

Background Plant hormones profoundly influence cotton growth, development, and responses to various stresses. Therefore, there is a pressing need for an efficient assay to quantify these hormones in cotton. In this groundbreaking study, we have established QuEChERS-HPLC‒MS/MS method, for the simultaneous detection of multiple plant hormones in cotton leaves, allowing the analysis and quantification of five key plant hormones. Results Sample extraction and purification employed 0.1% acetic acid in methanol and C18 for optimal recovery of plant hormones. The method applied to cotton demonstrated excellent linearity across a concentration range of 0.05–1 mg·L −1 , with linear regression coefficients exceeding 0.99. The limits of quantification (LOQs) were 20 μg·kg −1 for GA 3 and 5 μg·kg −1 for the other four plant hormones. Recovery rates for the five plant hormones matrix spiked at levels of 5, 10, 100, and 1000 μg·kg −1 were in the range of 79.07% to 98.97%, with intraday relative standard deviations (RSDs) ranging from 2.11% to 8.47%. The method was successfully employed to analyze and quantify the five analytes in cotton leaves treated with plant growth regulators. Conclusion The study demonstrates that the method is well-suited for the determination of five plant hormones in cotton. It exhibits excellent selectivity and sensitivity in detecting field samples, thus serving as a robust tool for in-depth research into cotton physiology.

研究领域: 农业化学 · 植物生理学 · 分析化学
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JOURNAL OF PHARMACEUTICAL SCIENCES · 2021 · IF 3.534

Enantiomeric Separation of Dioxopromethazine and its Stereoselective Pharmacokinetics in Rats by HPLC-MS/MS

Jia Lun,Wenying Zhang,Yu Zhao,Yongbo Song,Xingjie Guo

Dioxopromethazine (DPZ) is a popular phenothiazine antihistamine that is widely used as a racemic drug in clinical to cure respiratory illness. In our work, a reliable, specific, and rapid enantioselective HPLC-MS/MS method has been established and fully validated for the quantification of R- and S-DPZ in rat plasma. After plasma alkalization (with 1 M Na 2 CO 3 ), DPZ enantiomers and diphenhydramine (IS) were extracted using ethyl acetate. Completely separation of R- and S-DPZ (Rs = 2.8) within 12 min was implemented on Chiralpak AGP column (100 × 4.0 mm i.d., 5 μm) employing ammonium acetate (10 mM; pH 4.5) - methanol (90:10, v / v ) as mobile phase. Themultiple reaction monitoring (MRM) mode was used for the detection of DPZ enantiomers and IS. The transitions of m/z 317.2 → 86.1 and 256.2 → 167.1 werechosen for monitoring DPZ enantiomers and IS, respectively. Good linearity (r 2 > 0.995) was achieved for each DPZ enantiomer over the linear ranges of 1.00 - 80.00 ng/mL, with the lower limit of quantitation (LLOQ) of 1.00 ng/mL. The intra-day and inter-day precisions (RSDs,%) were below 12.3%, and accuracies (REs,%) were in the scope of-10.5% to 6.6%, which were within the admissible criteria. The validated bioanalytical approach was applied to the stereoselective pharmacokinetic (PK) research of DPZ in rat plasma for the first time. It was found that significant differences ( p < 0.05) exist between the main PK parameters of R- and S-DPZ, indicating the pharmacokinetic behaviors of DPZ enantiomers in rats were stereoselective. The chiral inversion of the enantiomers did not occur during the assay.

研究领域: 药物分析 · 药代动力学 · 生物分析
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MICROCHEMICAL JOURNAL · 2022 · IF 5.304

Determination of synthetic estrogens in milk by a novel hyper-crosslinked polymer SPME coupled with HPLC-MS

Tong Liao,Jia Jia,Kang Tong,Jiuhong Ouyang,Wei Jiang,Xia-ping Zhu

A novel hyper-crosslinked 2, 8, 14, 20-tetraphenyl calix [4] resorcinol arene polymer (HCP-TCRA) was synthesized by using an external crosslinking of 2, 8, 14, 20-Tetraphenyl calix [4] resorcinol arene (TCRA) as monomers and dimethoxymethane as crosslinker. The HCP-TCRA was explored as a SPME fiber coating material. A variety of physicochemical characterization demonstrated that the material has excellent chemical/thermal stability and strong hydrophobicity. The fiber demonstrated fantastic adsorptive property for three synthetic estrogens (diethylstilbestrol, hexestrol, ethinyloestradiol, abbreviated to SESs). In this work, an efficient HCP-TCRA fiber-based SPME method was developed to analyze SESs by coupling with HPLC-MS detection. Under the optimized SPME conditions, this method was shown a wide range of linearity (2.0–100.0 ng mL −1 for diethylstilbestrol, 1.0–100.0 ng mL −1 for hexestrol, and 30.0–480.0 ng mL −1 for ethinyloestradiol), low limits of detection (LODs, 0.5 ng mL −1 for DES 0.3 ng mL −1 for HEX, 10.0 ng mL −1 for EES) and fine reusability (more than 30 times). Finally, the proposed methods had been applied to the determination of SESs in milk samples with a simple pretreatment. At three different levels, relative recoveries presented between 86.7 and 106.4%. The method put up highly sensitive and budget-friendly   in detection SESs, and has capacity in quality control of milk products.

CAS / MDL: 56-53-1
研究领域: 分析化学 · 食品安全 · 环境科学
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ANALYST · 2019 ·Vol. 144 ·期 23 ·6981-6988 · IF 4.019

A HPLC-MS method for profiling triterpenoid acids and triterpenoid esters in Osmanthus fragrans fruits

Xiaoyan Liao,Fangli Hu,Zilin Chen

Triterpenoids, as an important family of plant secondary metabolites, have important biological activities associated with health and disease prevention. In this work, we proposed a HPLC-MS method for profiling multiple groups of triterpenoid acids and triterpenoid esters differing only in one position of the hydroxyl or methyl group in O. fragrans fruits. A total of thirty-one compounds were identified, and twenty-seven components were discovered in O. fragrans fruits for the first time. The HPLC-MS profiling method was applied in the analysis of the triterpenoids of O. fragrans flowers, and the time courses of triterpenoids of O. fragrans fruits.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 植物化学 · 植物代谢组学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2014 · IF 2.694

Pharmacokinetic study of multiple active constituents from Kushen–Gancao Decoction after oral administration in rat by HPLC–MS/MS

Qinhui Wang,Lei Shi,Xiuling Tang,Qingwei Wang,Xueliang Dang,Yan Zhang

Kushen–Gancao Decoction (KGD) is a classic traditional Chinese herb combination in treating viral hepatitis and chronic liver diseases. This study aims to investigate the pharmacokinetic (PK) study of matrine (MT), oxymatrine (OMT), glycyrrhizic acid (GL) and glycyrrhetinic acid (GA) following oral administration of KGD in rats. A rapid, sensitive and reliable HPLC–MS/MS method was successfully developed for the simultaneous determination of MT , OMT, GL and GA in rat plasma. A Inertsil C 18 analytical column was used with a gradient mobile phase system of methanol-ammonium acetate (5   mM) with a flow rate of 0.5   mL/min. The analysis was performed on a positive and negative ionization electrospray mass spectrometer via multi reaction monitoring (MRM). Linear calibration curves were obtained for the following concentration range: 10–5000   ng/mL for MT, OMT and GL, 50–15,000   ng/mL for GA in rat plasma ( R 2   >   0.99). The lower limit of quantification (LLOQ) was 5   ng/mL (MT, OMT and GL) and 20   ng/mL (GA). The intra- and inter-day accuracies ranged from −7.91 to 9.10% and precisions (RSD) were within 15%. The analytes were found to be stable under short-term temperature conditions, post-preparative temperature conditions, and after three freeze-thaw cycles conditions. The validated method was successfully applied to a pharmacokinetic study in rats after oral administration of KGD.

研究领域: 中药学 · 药理学 · 分析化学
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CHROMATOGRAPHIA · 2021 ·Vol. 84 ·期 11 ·1057-1064 · IF 2.044

Combination of Derivatization–HPLC–MS and Enzymatic Hydrolysis–Edman Degradation for Amino Acid Sequence and Configuration of Polymyxin B Components

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.

CAS / MDL: 632-20-2 319-78-8
研究领域: 生物化学 · 药物分析 · 微生物学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2023 · IF 3

Simultaneous quantification of donafenib, sorafenib, and their N-oxide metabolites in rat plasma using a HPLC-MS/MS method

Yutao Lou,Zhiyong Sun,Yitao Chai,Hui Qin,Qing Hu,Yujia Liu,Xiaowei Zheng,Ying Hu,Meihua Bao,Jinping Gu,Yiwen Zhang

Donafenib and sorafenib are small molecule chemotherapy drugs for the management of hepatocellular carcinoma, with donafenib being a deuterated derivative of sorafenib. To date, a high liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method that quantify donafenib, sorafenib, and their main metabolites has not yet been developed. The objective of this study was to establish a HPLC-MS/MS method for the simultaneous detection of donafenib, donafenib-N-oxide, sorafenib, and sorafenib-N-oxide and for the pharmacokinetic studies in rat. The extraction of all analytes was achieved by simple protein precipitation utilizing acetonitrile. The Waters XBridge C 18 column (2.1 × 100 mm, 3.5 µm) was selected, and the analytes could be efficiently separated and quantitated during a 2.8 min gradient elution procedure. The method was linear within the predefined quantification ranges and provided acceptable precision (%CV < 9.4%), reproducible extraction recovery (99.4%–111.5%), and low matrix effect (88.1%–98.6%). The hemolysis effect did not interfere with the quantification of all analytes, and similar results were obtained by changing the anticoagulant K 2 -EDTA to heparin or sodium citrate. Plasma pharmacokinetics revealed that the values of t 1/2 , C max , and AUC 0-t of donafenib were 1.4-, 6.2-, and 3.1-fold higher than those of sorafenib, respectively. In conclusion, the proposed bioassay was successfully applied to pharmacokinetic studies in rat after administration of donafenib and sorafenib. Our work not only improves the bioanalytical method for determining the plasma concentrations of donafenib, sorafenib, and their N-oxide metabolites, but also provides a scientific reference for clinical pharmacokinetic studies.

研究领域: 药物化学 · 临床药理学 · 分析化学
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2023 · IF 4.3

Quantification of cow milk in adulterated goat milk by HPLC-MS/MS using N-acetylglucosamine as a reliable biomarker of cow milk

Jing-Yan Li,Qian Ge,Bin Liu,Zhen-Peng Gao,Chun-Feng Guo

This study aimed to develop a non-protein-based method for quantify cow milk in adulterated goat milk. The raw cow milk and raw goat milk samples were mixed separately with the same volume of cold acetone and centrifuged to remove their proteins. The supernatants were evaporated, and the residues were derivatized by silylation followed by GC-MS analysis. N-acetylglucosamine was identified as a thermostable non-protein biomarker of cow milk. Its concentration in the raw cow milk (146.7 mg/L) was 32 times higher than that in the raw goat milk. On this basis, a HPLC-MS/MS method using positive-ion electrospray ionization in parallel reaction monitoring mode was developed for quantifying cow milk in adulterated goat milk by determining peak area of the biomarker. The method showed good linearity over cow milk concentrations of 1–100% and could detect as low as 0.3% cow milk in adulterated goat milk. Besides, the method was characterized by a simple sample pretreatment process, rapid detection, high accuracy, and high precision. With this method, a sample could be analyzed in 10 min. The present study demonstrated the feasibility of quantifying cow milk in adulterated goat milk using N-acetylglucosamine as a biomarker of cow milk.

研究领域: 食品科学 · 分析化学
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JOURNAL OF AOAC INTERNATIONAL · 2020 ·Vol. 104 ·期 2 ·479-484 · IF 1.51

A Simple and Standardized Method for the Determination of Total Solanesol in Potato Leaves and Its Extracts Based on HPLC-MS

Lan Tao,Yu Congcong,Li Ren,Ma Zheng,Xi Xingjun,Chu Qiao

BackgroundSolanesol is an important pharmaceutical intermediate raw material, mainly used to synthesize coenzyme Q10, vitamin K2. It can be found prominent in potato stems and leaves. But now potato stems and leaves are always abandoned or discarded as they are not suitable for use as feed in aquaculture or other purposes. These agricultural waste resources can be reutilized as the corresponding extracts.ObjectiveTo develop a simple and standardized method for the detection of total solanesol in potato leaves and its extracts.MethodsN-hexane was chosen as the extraction solvent for three times in the solanesol extraction from potato leaves. HPLC-MS was used for the detection.ResultsThe LOQ was 0.3 µg/g and the linear range was from 0.1  to 50 µg/mL. The precision and stability were evaluated by the relative standard deviations (RSDs) of three samples (potato leaves, Extract-1, Extract-2) for interday and intraday. The accuracy of the method was evaluated by the recoveries of three different spiked concentrations of solanesol for three samples, and results showed it ranged from 80.7% to 99.0% with RSDs less than 8.7%.ConclusionsThe method we established can provide a simple and standardized way for the extraction and detection of total solanesol.HighlightsThe work laid a foundation for the resource reutilization of potato stem and leaf.

研究领域: 植物化学 · 分析化学 · 药用植物学
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