FOOD CONTROL
·
2022
·
IF 6.652
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.
研究领域:
分析化学
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食品安全
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食品科学
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产品关联
DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2022
·
IF 4.52
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
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分析化学
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药学
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DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2023
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IF 4.3
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
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分析化学
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产品关联
DOI
高影响因子
Journal of Cotton Research
·
2024
·Vol. 7
·期 1
·1-14
·
IF 3.1
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
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植物生理学
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分析化学
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL SCIENCES
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2021
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IF 3.534
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
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药代动力学
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生物分析
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2014
·
IF 2.694
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
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药理学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2023
·
IF 3
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
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临床药理学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2023
·
IF 4.3
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
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分析化学
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DOI
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2018
·
IF 3.909
Baolei Fan,Tingting Li,Xiaofang Song,Chao Wu,Chunqi Qian
A specific HPLC-MS/MS (High-Performance Liquid Chromatography with tandem Mass Spectrometry) method was developed and validated for simultaneous determination of several monosaccharides in three kinds Osmanthus fragrans Lour . After extraction, separation, protein removal, pigment removal and hydrolysis , monosaccharides was finally obtained from Osmanthus fragrans Lour . Positive ion mode detection and Multiple Reaction Monitoring (MRM) mode were used for quantitative analysis by PMP pre-column derivatization and Electrospray Ionization (ESI). Analysis and content determination of 6 monosaccharide components in 3 kinds of Osmanthus fragrans Lour . The HPLC separation was achieved on a Shim-pack VP-ODS6022748 (150 L × 2.0) with gradient elution at a flow rate of 0.2 ml/min in a run time of 40 min, and the mobile phase was acetonitrile-5 mmol/L ammonium acetate. PMP derivatization in HPLC-MS/MS can accurately measure Osmanthus fragrans Lour . mannose (Man), ribose (Rib), rhamnose (Rha), galacturonic acid (Gal UA), glucose (Glu), galactose (Gal), xylose (Xyl), fucose (Fuc). The results showed that HPLC-MS/MS pre-column derivatization method was simple and rapid, with small measurement error, but high sensitivity and good repeatability. The analysis of monosaccharide components in polysaccharide components has important practical significance.
研究领域:
植物化学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2021
·Vol. 44
·期 9
·1852-1865
·
IF 3.645
Jingjing Wu,Song Zhang,Jiali Li,Xiaoli Zhong,Guiping Feng,Liangqing Hu,Fan He,Hanjing Cen,Yilu Chen,Yanling He,Huasong Zeng,Xiao Chen,Xiaolan Mo
Low-dose methotrexate is the first-line therapy for juvenile idiopathic arthritis. In vivo, methotrexate is converted into a series of methotrexate polyglutamates whose intracellular levels contribute significantly to its efficacy and toxicity. In this study, a novel high-performance liquid chromatography–tandem mass spectrometry method was developed and validated to simultaneously determine erythrocyte methotrexate polyglutamates using stable isotope-labeled internal standards. Erythrocyte samples were precipitated by perchloric acid and then determined on an XBridge BEH C18 column with an XP vanguard precolumn in 12 min. The mobile phase consisted of 10 nM ammonium acetate (pH 10) and methanol under gradient elution. The detection was carried out in multiple reaction monitoring mode via an electrospray ionization source in positive ionization mode. The calibration curve for each metabolite was linear from 2.0 to 500.0 nmol/L ( r 2 > 0.99). The intraday and interday accuracies were between 93.0 and 107.0%, and the corresponding precisions were between 0.8 and 5.2%. The relative recovery ranged from 82.7 to 105.1%, and the relative matrix effect varied from 96.5 to 104.4%. The erythrocyte metabolites were stable for 30 days at −80°C. This simple and accurate method is applicable to routine monitoring of the concentration of erythrocyte methotrexate polyglutamates in patients to achieve individualized treatment.
研究领域:
药理学
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分析化学
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临床医学
✓ 已验证
DOI
PubMed
高影响因子
ACS Omega
·
2021
·
IF 3.512
Zhihui Lin,Yingnan Lin,Jianqi Lin,Yizhi Zhang,Song Fang
A modified QuEChERS method in combination with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was first developed for the determination of fenbutatin oxide in six types of samples (soil, tobacco, rice, milk, pork liver, and pork). Fenbutatin oxide was extracted with acetonitrile containing 1% formic acid (v/v) and purified by dispersive solid-phase extraction using primary secondary amine (PSA) and quantitatively analyzed by HPLC-MS/MS. In the range of 0.005–1 mg/kg, a good linear relationship exists between the concentration of fenbutatin oxide and the peak area, giving a coefficient of determination (R2) of >0.99. The recoveries of fenbutatin oxide at three spiked levels were 79.04–97.12% with the relative standard deviations (RSDs) of 3.30–10.96%, and the limit of quantification (LOQ) was 0.007 mg/kg. In addition, the developed method is consistent with the reference method (R2 = 0.9896, n = 40). The method is demonstrated to be convenient and reliable for the routine monitoring of fenbutatin oxide in soil and plant- and animal-derived foods.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·
IF 3.8
Wu Jiaxin,Yao Shunying,Wang Yiwei,Fan Sai,Cui Xia,Chen Dawei,Shi Zhixiong
Organophosphate esters (OPEs) are commonly used chemicals and are also regarded as emerging environmental pollutants. Recently, it has been proved that metabolites of OPEs (mOPEs) could also cause health concerns. However, analytical methods for the concurrent measurement of OPEs and mOPEs in human matrices are still complicated. In this study, a convenient and efficient analytical method combining a cold-induced strategy and HPLC–MS/MS was developed to simultaneously determine 18 OPEs and 10 mOPEs in human serum, urine, and human milk. In brief, after the sample was extracted with acetonitrile, a “one-step” treatment combining purification and enrichment was accomplished by cold-induced liquid–liquid extraction (CI-LLE), and analytes were then quantified by HPLC–ESI–MS/MS. The ratio of acetonitrile/water, and the temperature and time set in the CI-LLE procedure were optimized for achieving the highest enrichment factors. Under the best conditions, linearity, limits of detection (LODs), recovery, precision, and matrix effects of OPEs/mOPEs were verified. LODs of OPEs/mOPEs in serum, urine, and human milk were 0.1–113 pg/mL, 0.1–22 pg/mL, and 0.2–22 pg/mL, respectively. Average recoveries ranged from 80 to 123%, with relative standard deviations lower than 15% for most analytes. The matrix effect test showed slight signal enhancement or inhibition, and the use of isotopically labeled internal standards (ISs) could compensate for the effects. In real sample analysis, both OPEs and mOPEs showed high detecting frequency, which indicated their ubiquity in humans.
研究领域:
环境科学
·
分析化学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）