JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Yirang Wang,Jingyi Fan,Xian Fang,Yue Zhuo,Siyan Xu,Lei Liao,Xiaojun Deng,Bing Liu
AICAR (5-amino-4-imidazolecarboxyamide ribonucleoside), as a metabolic modulator, is classified in the S4 category by the World Anti-Doping Agency (WADA). Carbon Isotope Ratio Mass Spectrometry (CIR) is the mainstream method for distinguishing the endogenous and exogenous sources of AICAR in urine due to the significant individual difference in the concentration. The purpose of this study is to establish a gas chromatography combustion Isotope Ratio Mass Spectrometry (GC/C/IRMS) method for AICAR based on efficient two-dimensional liquid chromatography (2D-HPLC) separation. Method In this study, an automated 2D-HPLC separation technique was used to separate and purify AICAR and endogenous reference substances in urine samples. Then, AICAR was derivatized with 3-TMS as the main derivative product, while the endogenous reference compounds remained in their original form. Subsequently, the developed GC/C/IRMS method was utilized for the detection of the target and reference substances. Followed, we evaluated the applicability of this method using urine samples from two Asian males administered a low dose of AICAR (3 grams). Results The advantages of this study include: 1) reduced sample pretreatment time: the established 2D-HPLC separation method can separate the target and endogenous reference substances in one step; 2) low interference: the isotope chromatograms have low background interference, and the separation of endogenous reference substances is purer; 3) more accurate result calculations: this method only requires derivatization and result correction for AICAR, with the endogenous reference substances measured in their original form, reducing biases from corrections of multiple substances. The detection method performed well, with a concentriton limit of 2500 ng/mL, meeting the needs of routine detection concentrations. The CIR results from volunteer samples indicated that samples collected within 16 hours post-administration exceeded the threshold set in the literature. Conclusion This study successfully established a 2D-HPLC-GC/IRMS method that integrates CIR as the most stable indicator for distinguishing the internal and external sources of AICAR. After administering a low dose of AICAR to the Asian population, exogenous drug characteristics were manifested within 16 hours. This observation, when compared to the 40-hour detection window cited in the literature, suggests that the length of the detection window is positively correlated with the dosage of the test drug.
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RSC Advances
·
2025
·Vol. 15
·期 30
·24437
·
IF 4.6
Feng Wen,Yongjun Wu,Jing Jin,Lincheng Zhang,Shuoqiu Tong,Cen Li,Li Ran,Yuzhang Zhu
Fermented soybean products are an integral part of the Chinese diet, valued for their distinctive aroma. Bacillus subtilis ( B. subtilis ) BJ3-2 is a highly effective fermentation strain widely used in the industrial production of bacterial-type douchi. However, the specific aroma characteristics of soybeans fermented by this strain remain unclear. This study utilized gene knockout, GC-O-MS, and multivariate statistical analysis to comprehensively investigate the aroma components of soybeans fermented by B. subtilis BJ3-2. For the first time, 12 key aroma skeleton compounds were identified, including guaiacol, 2,5-dimethylpyrazine, and 2-methylbutyric acid, which primarily contribute to the smoky, roasted, and sweaty aroma attributes of fermented soybeans. Additionally, 17 compounds were considered to have important coordinating effects on soybean aroma, such as 3-hydroxy-2-butanone (buttery, creamy). Partial least squares regression (PLSR) analysis demonstrated a good correlation between key aroma compounds and sensory attributes. Gene knockout of fadA and bkdB resulted in a significant increase in 2,5-dimethylpyrazine and 1-octen-3-ol levels, along with a marked reduction in 2-methylbutyric acid levels. These changes enhanced the roasted and beany notes, reduced the sweaty aroma, and ultimately improved the overall aroma profile. These findings provide insights into the genetic regulation of aroma in fermented soybean products and form a foundation for reducing undesirable aromas and improving the overall aroma quality of industrially produced douchi. Bacillus subtilis fermented soy food is deeply loved by consumers, and its unique aroma characteristics are influenced by the fadA and bkdB genes.
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LWT-FOOD SCIENCE AND TECHNOLOGY
·
2026
·
IF 7.1
Jianya Cai,Wenyan Ma,Tingting Xu,Ye Ke,Hanbin Chen,Ziyang Wu,Shuangta Xu
Freeze-dried shrimp retained 575 g/kg umami intensity and 6.57 mg/kg iodide. • Infrared-dried shrimp scored highest in overall liking (8.19 on a 10-point scale). • Thirty key odorants distinguished the four dried-shrimp aroma styles. • Sun-dried shrimp held the least iodide (1.15 mg/kg) and the most rancid notes. • Hot-air drying produced the strongest roast notes yet depleted iodide and umami. This study investigated the effects of four drying methods, hot-air drying (HAD), sun drying (SD), vacuum freeze-drying (VFD), and infrared radiation drying (IRD), on flavor quality and iodine nutritional characteristics of dried shrimp ( Fenneropenaeus chinensis ) using a multi-dimensional flavoromics approach. HS-SPME-GC-O-MS with aroma extract dilution analysis (AEDA) identified 94 volatile compounds, from which 30 key odorants (OAV ≥ 1, FD ≥ 64) were quantified by stable isotope dilution assay. OPLS-DA (R 2 Y = 0.97, Q 2 = 0.94) discriminated the four groups, with dimethyl trisulfide (VIP = 3.49) and 2,3,5-trimethylpyrazine (VIP = 3.39) as core markers for VFD and HAD, respectively. Aroma recombination and omission experiments validated the identification completeness. VFD maximized freshness retention (EUC = 575 g MSG/kg) and iodine preservation (6.57 mg/kg; iodide/total iodine = 0.615), yet its sensory acceptability (6.33/10) was inferior to IRD (8.19) and HAD (7.37) due to lacking roasted complexity. EEG olfactory perception confirmed that IRD elicited the most balanced cortical response with the highest alpha-band power (12.23 μV 2 /Hz). A fundamental trade-off exists among freshness retention, roasted aroma development, and iodine preservation, with no single method dominating all dimensions. IRD is recommended as the optimal industrial drying method, achieving the best three-dimensional quality balance. Download: Download high-res image (498KB) Download: Download full-size image
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FOOD CHEMISTRY
·
2015
·
IF 3.391
Yunzi Feng,Yu Cai,Dongxiao Sun-Waterhouse,Chun Cui,Guowan Su,Lianzhu Lin,Mouming Zhao
Aroma extract dilution analysis (AEDA) is widely used for the screening of aroma-active compounds in gas chromatography–olfactometry (GC–O). In this study, three aroma dilution methods, (I) using different test sample volumes, (II) diluting samples, and (III) adjusting the GC injector split ratio, were compared for the analysis of volatiles by using HS-SPME–AEDA. Results showed that adjusting the GC injector split ratio (III) was the most desirable approach, based on the linearity relationships between Ln (normalised peak area) and Ln (normalised flavour dilution factors). Thereafter this dilution method was applied in the analysis of aroma-active compounds in Japanese soy sauce and 36 key odorants were found in this study. The most intense aroma-active components in Japanese soy sauce were: ethyl 2-methylpropanoate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, ethyl 4-methylpentanoate, 3-(methylthio)propanal, 1-octen-3-ol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2-methoxy-4-vinylphenol, 2-phenylethanol, and 4-hydroxy-5-ethyl-2-methyl-3(2H)-furanone.
研究领域:
食品科学
·
分析化学
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BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 3
·e4748
·
IF 1.748
Chu Liu,Xiangyong Yu,Zhaorui Meng,Ning Zhao,Fujuan Bai,Longshan Zhao
A simple and efficient method involving microwave-assisted extraction (MAE) combined with GC–MS was established to determine 1,3-di- tert -butylbenzene (DBB), 2,4-di- tert -butylphenol (DBP), 3,5-di- tert -butyl-4-hydroxybenzaldehyde (DBHBA) for evaluating the compatibility of antimicrobial peptide PL-5 spray with drug-packaging materials. In this study, the antimicrobial peptide PL-5 spray was purified using a Welchrom C18 column, and the high-density polyethylene spray bottle with liquid collection tube was first mixed with absolute ethanol, which would be subjected to MAE for further measurement by GC–MS. Various experimental parameters were systematically optimized, and good linearities were obtained within the range of 0.05–1.00 μg/mL for DBB and DBHBA and 0.50–10.00 μg/mL for DBP, with limits of detection (LODs) of 0.99 ng/mL (DBB), 16.34 ng/mL (DBP), and 1.64 ng/mL (DBHBA). Satisfactory recoveries that ranged from 96.0% to 107.2% were acquired, and the relative standard deviation was ≤ 4.7%. The results showed that the maximum daily usage of DBB, DBP, and DBHBA was 9.859, 163.445, and 16.399 ng, respectively, which was far below the corresponding permitted daily exposure values according to the safety assessment, indicating that the migration of analytes did not bring any potential safety risk. The compatibility between the drug and the packaging materials was favorable.
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Analytical Methods
·
2024
·
IF 2.7
Hongxu Zhou,Qing Jiang,Xin He,Xian Fu,Jun-Yan Liu
Fatty acids (FAs) are essential molecules in all organisms and are involved in various physiological and pathophysiological processes. Pentafluorobenzyl bromide (PFBBr) is commonly used for FAs derivatization for gas chromatography-mass spectrometry (GC–MS) quantification by chemical ionization (CI). While CI is the conventional ionization mode for PFBBr derivatization, electron ionization (EI) source has also demonstrated efficacy in achieving satisfactory analytical performance for the analysis of PFB esters. In this study, we present a novel approach utilizing PFBBr-derivatization on a GC-EI-MS platform to quantitatively analyze a comprehensive range of 44 fatty acids (FAs) spanning from C2 to C24. The method's sensitivity, precision, accuracy, linearity, recovery, and matrix effect were rigorously validated against predetermined acceptance criteria. In comparison to the conventional CI ionization mode, the utilization of PFBBr-derivatization in GC-EI-MS exhibits a wider range of applications and achieves comparable sensitivity levels as the conventional CI platform. By using this method, we successfully quantified the 44 FAs in plasma and feces samples from the mice with deoxynivalenol (DON)-induced kidney injury. Among these, the levels of most FA species were increased in the DON-exposure group compared with the control group. The orthogonal partial least squares discriminant analysis (OPLS-DA) of all the tested FAs showed a visual separation of the two groups, indicating DON exposure resulted in a disturbance of FA profile in mice. These results indicate that the established method by integration of GC-MS with PFBBr derivatization is an efficient approach to quantify the comprehensive FA profile, which includes short-, medium- and long-chain FAs. In addition, our study provides new insights into the mechanism underlying DON exposure-induced kidney injury.
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MOLECULES
·
2014
·Vol. 19
·期 4
·4857-4879
·
IF 2.095
Chen Li,Feng Xu,De-Mei Xie,Yu Jing,Ming-Ying Shang,Guang-Xue Liu,Xuan Wang,Shao-Qing Cai
Traditional Chinese Medicine (TCM) nasal therapy has been utilized to treat numerous diseases for over two millennia. It has many advantages compared with other routes. In this article, headspace-solid phase microextraction-gas chromatography-mass spectrometry and high performance liquid chromatography-atmospheric pressure chemical ionization-ion trap-time of flight-multistage mass spectrometry were applied for the first time to analyze the absorbed constituents in rabbit plasma and cerebrospinal fluid (CSF) after intranasal administration of Asari Radix et Rhizoma (AR). In total, 47 absorbed AR constituents including 14 monoterpenes, 10 phenylpropanoids, four benzene derivatives, two alkanes, nineN-alkylamides and eight lignans were tentatively identified in the rabbit plasma and CSF. Thirty-three absorbed constituents are found to have different bioactivities related to the pharmacological actions of AR through bibliography data retrieval. These indicated that many types of constituents of TCM can be absorbed at the nasal cavity into both rabbit blood and CSF. This is the first study to explore the absorption of AR, and comprehensively analyze the absorbed constituents after intranasal administration of TCM. These findings extend our understanding of the effective substances of AR, and inspire us to make a hypothesis on the mechanism of additive effect of multiple constituents of TCMs, which is very worthy of further investigation.Keywords:nasal therapy;Asarum heterotropoidesvar.mandshuricum;intranasal administration;effective substance;cerebrospinal fluid;absorption;SPME;GC-MS;LC-MS;additive effect
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Lipids in Health and Disease
·
2024
·Vol. 23
·期 1
·1-15
·
IF 3.9
Guo XiaoYu,Zhou Jianglu,Yu Hong,Cao Han,Li Xia,Hu Qing,Yu YunQiu
Background Long-chain fatty acids (LCFAs) are involved in regulating multiple physiological processes as signalling molecules. Gas chromatography–mass spectrometry (GC–MS) is widely used to quantify LCFAs. However, current quantitative methods for LCFAs using GC–MS have demonstrated complicated issues. Psoriasis is a chronic inflammatory skin disease, and its pathogenesis may be related to the overproduction of interleukin-17A (IL-17A). Clinical efficacy of anti-IL-17A monoclonal antibody (mAb) treatment in psoriasis patients has been demonstrated. Recent studies suggest that LCFAs play varying roles in the pathogenesis of psoriasis. However, more comprehensive research is needed to illuminate the mechanism of LCFAs in psoriasis. Methods The established in situ derivatization method for analysing LCFAs with a GC–MS platform was utilized to conduct serum lipidomics analysis of healthy volunteers and psoriasis patients receiving pretherapy and posttreatment with of anti-IL-17A mAb. Imiquimod (IMQ)-treated wild type (WT) and T-cell receptor delta chain knock-out ( Tcrd −/− ) mice were used to investigate the correlation between IL-17A and abnormal changes in LCFAs in psoriasis patients. Results A rapid and sensitive in situ extraction derivatization method for quantifying LCFAs using GC–MS was established. Serum lipidomic results showed that psoriasis patients had higher levels of saturated fatty acids (SFAs) and ω-6 polyunsaturated fatty acids (PUFAs) but lower levels of monounsaturated fatty acids (MUFAs) and ω-3 PUFAs than healthy individuals, indicating impaired serum LCFA metabolism. Anti-IL-17A mAb treatment affected most of these LCFA changes. Analysis of LCFAs in IMQ-treated mice showed that LCFAs increased in the serum of WT mice, while there were no significant changes in the Tcrd −/− mice. SFAs increased in IMQ-treated WT mice, while MUFAs showed the opposite trend, and PUFAs did not change significantly. Conclusions This study presented a dependable method for quantifying LCFAs that enhanced sensitivity and reduced analysis time. The lipidomic analysis results showed that anti-IL-17A mAb not only ameliorated skin lesions in psoriasis patients but also affected abnormal LCFAs metabolism. Furthermore, the study indicated a potential correlation between IL-17A and abnormal LCFA metabolism in psoriasis patients, which was supported by the alterations in serum LCFAs observed in IMQ-treated WT and Tcrd −/− mice.
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Yiheng Li,Xue Yang,Qimin Zhang,Longlin Wang,Huiyuan Guo,Xuhui Chen,Yantao Guo,Xiuping Li,Weibing Zhang,Pengjie Wang,Pengcheng Wen
Zhaiji millet vinegar (ZJMV) is a traditional grain-fermented condiment whose quality improvement is associated with aging time. This study revealed the evolution of physicochemical properties and whole-component of ZJMVs aging 2 to 10 years. Results demonstrated pH, chroma, and the content of total acid, reducing sugar, and amino acid nitrogen fluctuate dynamically, while antioxidant activities were significantly correlated with the content of total flavonoids, total phenols, tetramethylpyrazine, amino acids, and organic acids ( p < 0.05). GC-IMS and metabolomics identified 47 volatile organic compounds (VOCs) and 6530 metabolites, with 6 differential VOCs and 19 differential metabolites ( p < 0.05, variable importance in projection (VIP) > 1, fold change (FC) < 0.5 or > 2) being shared aging markers. KEGG pathway analysis indicated amino acid metabolism enriched the most differential metabolites, whereas biosynthesis of various alkaloids was critical. Our findings provide novel mechanistic insights into the quality development of ZJMV during aging.
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INTERNATIONAL JOURNAL OF MASS SPECTROMETRY
·
2020
·
IF 2.09
Jiaxing Fan,Jianglu Zhou,Shenmin Su,Yunqiu Yu,Lihong Chen,Yunchen Le,Xiaopan Wang,Li Zhang,Jie Zheng,Xia Li
Psoriasis is a common chronic inflammatory skin disease which may exhibit a variety of skin clinical manifestations associated with multiple comorbidities. However, its pathogenesis associated with metabolism has not yet been understood. The metabolites of tricarboxylic acid (TCA) cycle and amino acids are interlinked with each other and involve many physiological processes. This study determined 32 metabolites of TCA cycle and amino acids in psoriasis using an improved GC-MS method. This one-pot derivatization applied silanization and oximation simultaneously for easy, quick and sensitive quantitative detection of 32 metabolites in serum of patients with psoriasis. Through the established GC-MS method, 32 metabolites in serum were detected in a single run. The result of this preliminary study showed that there were significant alterations of the metabolites in tricarboxylic acid (TCA) cycle and amino acids before and after treatment. A shift towards healthy controls of these metabolites after treatment was observed using principal component analysis (PCA) as well. Receiver operating-characteristic curve (ROC) analysis of the analyzed 32 metabolites filtered 5 potential biomarkers of the clinical efficacy of the treatment. This result suggested the importance of these metabolites in the pathogenesis of psoriasis. To our best know, this is the first targeted metabolomics work to study the changes of TCA cycle metabolites and amino acids in the background of treatment of psoriasis.
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FOOD CHEMISTRY
·
2024
·
IF 8.5
Ligang Yu,Ying Pang,Guang Shen,Baoqing Bai,Yukun Yang,Maomao Zeng
This work aimed to investigate the effects of frozen storage on volatile compounds of white meats (chicken and duck) and red meats (pork, beef, and mutton). The samples were stored at −18 °C for 0, 2, 4, 10, 18 weeks, and volatile compounds were analyzed by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry. Results indicated that the total amounts of volatile compounds increased with frozen storage duration of meats. The correlations were observed between frozen storage duration and levels of 2-ethyl-1-hexanol, tetradecane, nonanal, decanal, octanal, tridecanal, benzaldehyde, pentadecane, propanoic acid,2-methyl-,3-hydroxy-2,2,4-trimethylpentyl ester, heptadecane, and hexanal ( r = 0.7456–0.9873). Levels of octanal and propanoic acid,2-methyl-,3-hydroxy-2,2,4-trimethylpentyl ester in white meat and benzaldehyde in red meat versus frozen storage duration fitted very well with zero-order reactions. Therefore, it was concluded that changes in volatile compounds derived from lipid oxidation may be used as indicators of quality deterioration during frozen storage of meat.
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Food Bioscience
·
2025
·
IF 5.9
Lu Feng,Jingxia Yang,Liping Sun,Xiaoyan Zhu,Wei Lan,Guangqing Mu,Xuemei Zhu
We evaluated the changes in volatile and nonvolatile flavor substances after fermented milk was fermented by Lacticaseibacillus rhamnosus WH. FH-19 using Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS) and High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS). The results have shown that the addition of L. rhamnosus WH. FH-19 can increase the contents of acetoin and 2-nonanone which can give fermented milk cream and cheese flavor, and significantly enrich amino acid metabolism and carbon metabolism. The fermentation of L. rhamnosus WH. FH-19 increased the contents of L-glutamic acid, taurine, stachyose, erythritol, L-rhamnose, retinol, pantothenic acid and 19 oligopeptides in fermented milk, and endowed fermented milk with good flavor, quality and antioxidant capacity. The results presented that L. rhamnosus WH. FH-19 can increase the content of flavor substances, promote the metabolism of amino acids and carbohydrates in fermented milk, and produce more antioxidant metabolites, which had the potential as a starter of fermented milk.
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