FOOD CHEMISTRY
·
2023
·
IF 8.8
Haiyue Yuan,Bei Li,Jing Wei,Xiaowei Liu,Zeying He
In this study, multi-residue analysis methods for 32 pyrethroids in fruit and vegetable samples were established in both GC–MS/MS and UHPLC-MS/MS. The parameters that affecting the ionization efficiencies of pyrethroids in UHPLC-ESI-MS/MS, including ion source temperature, in-source fragmentation, and mobile phase conditions were thoroughly investigated to guarantee better performance. These two techniques were comprehensively compared in terms of recovery, LOQ, linearity, and matrix effects. In general, UHPLC-MS/MS was found suitable for more pesticides than GC–MS/MS. Lower LOQs were obtained for most of the selected pyrethroids in UHPLC-MS/MS. Similar results were obtained in terms of recoveries and RSDs for the validated pesticides in fortification experiments. A total of 136 real samples were analyzed by both techniques, obtaining similar results. The results suggest that UHPLC-MS/MS offers a suitable alternative to GC–MS/MS in the routine analysis of pyrethroids in fruits and vegetables.
研究领域:
分析化学
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环境科学
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农业化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yuxia Shen,Wei Xiong,Qiqin Wang,Wentian Zhang,Hongzhen Xie,Yuting Cao,Qing Xu,Luhong Wen,Ning Gan
In this work, a disposable and inexpensive bamboo stir bar containing an organic membrane was constructed to perform stir bar sorptive extraction (SBSE), followed by portable mass spectrometry to achieve on-site detection of four residual drugs (malachite green, crystal violet and their metabolites) in fishes. The entire method uses only microliter quantities of organic solvents, enabling environmentally friendly pretreatment. The portable mass spectrometer can simultaneously detect four target analytes in a sample in approximately ten seconds. Under the optimal conditions, the proposed method was successfully applied to simultaneously detect four drugs in fish samples with detection limits of 0.16-0.59 µg/kg. The spiked recoveries for mandarin fish and lateolabrax maculatus were 74.5-96.5%, with relative standard deviations (RSD) of 4.4-16%. In addition, the matrix effects of the four analytical targets in the method were experimentally verified to range from 7.30% to 20.62%. The method can potentially be extended to the on-site detection of other veterinary drug residues in foods.
研究领域:
分析化学
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环境科学
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食品安全
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兽医学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Xian Cheng,Yan-Ju Lu,Sheng-Nan Li,Ya-Zhou Xu,Pan-Pan Li,Jing Wang,Shi-Chao Xu,Yan Gu,Liang-Wu Bi,Yu-Xiang Chen
Fungicide residues in food can pose serious hazards to humans. The aim of this study was to establish a new method of semistable emulsion assisted dispersive liquid–liquid microextraction (DLLME) for the preconcentration and determination of fungicide residues in juice samples. In this study, Gum Acacia (GA) was selected as the dispersive agent and decanoic acid was adopted as the extractant in aqueous sample. Based on that, a semistable emulsion was induced to facilitate the extraction of target analytes and automatic phase separation. The mechanistic analysis results revealed that the formation of the semistable emulsion was attributed to the mild emulsification of GA with a high molecular weight. Besides, the semistable emulsiont allowed the automatic phase separation in DLLME for the first time. Moreover, the novel method was optimized for detecting fungicide residues and exhibited good linearity (R2 ≥ 0.995), precision (≤16.2 %), matrix effect (≤9.8 %), method recovery (84.0–103.6 %), as well as a low limit of detection (0.5–2.5 μg·L −1 ) and quantitation (1–5 μg·L −1 ). In conclusion, this method can be employed to effectively measure fungicide residues in juice samples (orange, grape, carrot and peach). Furthermore, this method can be considered as an effective DLLME alternative for the automatic pretreatment of samples, exhibiting a promising application prospect in food safety.
研究领域:
分析化学
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食品安全
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环境科学
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产品关联
DOI
高影响因子
Chinese Journal of Chromatography
·
2022
·Vol. 40
·期 5
·433-442
·
IF 0
Yangjie LI,Jiaying HUANG,Jihui FANG,Zhiye HUANG
A high throughput screening method based on ultra performance liquid chromatography-quadrupole-time-of-flight high resolution mass spectrometry (UPLC-Q-TOF HRMS) was developed for the simultaneous and rapid confirmation of 73 prohibited compounds in cosmetics. The sample was dispersed in a saturated sodium chloride solution and ultrasonically extracted using acetonitrile containing 0.2% (v/v) formic acid. The resultant solution was centrifuged and then cleaned using dispersive solid phase extraction using a primary secondary amine (PSA) sorbent. The purified solution was centrifuged, and the supernatant was filtered through a 0.22 μm membrane before determination. The optimal pretreatment method was determined by comparing the recovery rates obtained using different extraction solvents and different amounts of purifying agents. The chromatographic separation conditions and mass spectrometry scanning mode were also optimized. Chromatographic separation was performed on an Acquity UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with gradient elution using 0.1% (v/v) formic acid aqueous solution and methanol as mobile phases. The eluent from the column was further detected using Q-TOF HRMS with the high resolution multiple reaction monitoring (MRM HR) scanning mode. Retention time, precise mass of parent ion, isotope abundance ratio, and precise mass of fragment ions were the parameters considered for rapid untargeted screening and confirmation. The matrix effects of water- and cream-based cosmetics were investigated. The matrix effects could be addressed using the matrix matched standard curve method. The correlation coefficients for the 73 prohibited compounds were all >0.99 in the corresponding linear concentration range. The limits of detection (LODs) were in the range of 5-150 μg/kg, and the limits of quantification (LOQs) were in the range of 15-450 μg/kg. Average recoveries were in the range of 60.3%-130.3% at three spiked levels, and the intra-day and inter-day precisions were 0.8%-10.0% ( n =6) and 1.1%-15.0% ( n =3), respectively. A total of 692 cosmetics samples were screened; 16 positive samples were detected, namely, sulfamethoxazole, meprednisone, lincomycin, 4-acetamidophenol, trimethoprim, alfacalcidol, betamethasone 17-valerate, brimonidine, chloramphenicol, chlorpheniramine, clobetasol propionate, crotamiton, econazole, ketoconazole, prednisone 21-acetate, and prednisone, with content in the range of 0.5-1136.1 mg/kg. The optimized method is accurate, fast, and simple, and it is suitable for the routine detection and rapid screening of common prohibited compounds in cosmetics. In addition, a screening and confirmation library was established for the 650 prohibited compounds using SCIEX OS and Library View software, using information-dependent acquisition (IDA)-MS/MS mode for MS data acquisition. The database contains multiple types of information, including formulas, theoretical exact mass, retention time, precise mass of parent ion, isotope abundance ratio, and fragment ion distribution. The library can be used for the simultaneous and rapid confirmation of prohibited compounds in cosmetics.
研究领域:
分析化学
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化妆品科学
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药物分析
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毒理学
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产品关联
DOI
PubMed
JOURNAL OF HAZARDOUS MATERIALS
·
2023
·
IF 13.6
Man-Man Wang,Zi-Ling Li,Han Wu,Ke-Yan Chen,Fan Guo,Gui-Fu Zuo,Yu He,Xue-Bo Yin
Magnetic solid-phase extraction (MSPE) was developed based on a well-designed Fe 3 O 4 -NH 2 @g-C 3 N 4 nanocomposite as sorbent for a mixture of six benzophenones (BPs) in environmental water samples. The composite fabricated via in-situ self-assembled g-C 3 N 4 shell with homogeneous polymerization of cyanuric chloride and cyanuric acid on Fe 3 O 4 -NH 2 core. While high adsorption capacity was derived from g-C 3 N 4 via hydrophobic, π-π and hydrogen bonding interactions to the targets, the fast magnetic separation was realized with Fe 3 O 4 core for less solvent consumption. In combination with LC-MS/MS, the Fe 3 O 4 -NH 2 @g-C 3 N 4 sorbent minimized the interfering components, reduced the matrix effects, and provided the enrichment factors of 121–150 for six BPs with relative standard deviations ≤ 9.7% even after 20 times extraction-desorption cycles. The present method gave the detection limits of 0.3–2.5 ng/L for six BPs with the linear ranges of 1.0–2000 ng/L, and the recoveries of 84.6%−104% in sea water and 86.2%−107% in lake water samples. Thus, the Fe 3 O 4 -NH 2 @g-C 3 N 4 -based MSPE coupled with LC-MS/MS method provided a convenient, efficient, and reliable alternative to monitor trace BPs in environmental water samples.
研究领域:
环境科学
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分析化学
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材料科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2022
·
IF 5.895
Yaran Liu,Xu Qian,Jiangtao Xing,Na Li,Junlong Li,Qingyu Su,Yixin Chen,Bolin Zhang,Baoqing Zhu
This paper clarifies the contribution of lactones and volatile phenols to the aroma of nongrape wine. A target method for the simultaneous determination of these two kinds of volatiles in nongrape wines was developed using headspace-solid-phase microextraction (HS-SPME) combined with high-resolution gas chromatography-Orbitrap mass spectrometry (GC-Orbitrap-MS). A high-resolution mass spectrometry database including 12 lactones and 11 volatile phenols was established for qualitative accuracy. Different matrix-matched calibration standards should be prepared for specific samples due to the matrix effects. The method was successfully validated and applied in three nongrape wines. Hawthorn wine contained more lactones (δ/γ-hexalactone, δ/γ-nonalactone, δ/γ-decalactone, γ-undecalactone, δ/γ-dodecalactone, C10 massoia lactone, and whiskey lactone), while blueberry wine contained more volatile phenols (especially 4-vinylguaiacol and 4-ethylguiaiacol). Goji berry wines contained certain concentrations of δ-nonalactone, γ-nonalactone, δ-hexalactone, and 3-ethyl phenol. This study demonstrated that HS-SPME-GC-Orbitrap-MS can be applied for the accurate quantification of trace aroma compounds such as lactones and volatile phenols in fruit wines.
研究领域:
食品科学
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分析化学
·
农学
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DOI
PubMed
高影响因子
Analytical Methods
·
2021
·Vol. 13
·期 11
·1404-1411
·
IF 2.896
Wenxue Xu,Yufeng Hu,Minghuo Wu,Enming Miao,Hao Zhou,Xuwang Zhang,Jingjing Zhan
A method consisting of solid-phase isotope dansylation (derivatization with dansyl chloride) and liquid chromatography-high resolution mass spectrometry (LC-HRMS) was developed for the quantitative analysis of phenolic compounds (phenols) in environmental samples. A magnetic-HLB (hydrophilic lipophilic balanced) material was synthesized and applied as an adsorbent in magnetic solid-phase extraction (MSPE) for the enrichment of the analytical targets. Furthermore, with the solid-phase isotope labeling, the desalting and removal of labeling residuals could be simplified over conventional in-solution labeling. In addition to overcoming the matrix effect by isotope dansylation, the sensitivity for the analysis of phenols by LC-HRMS was remarkably improved by over 100-fold. The method was systematically verified, and good accuracy (86.5–104.9%) and precision (<8.6% and <11.4% for intra- and inter-day, respectively) were achieved for the tested 15 phenols. The limits of detection (LODs) of this method were estimated to be 0.2–5 ng L−1 and 5–100 ng kg−1 in estuary water and sediment samples, respectively. With this method, samples collected from the Daliao River estuary (Panjin, China) were analyzed. It was found that all of the targeted phenols were detected at concentrations ranging from unquantifiable to 485 ng L−1 (the total concentration of analytes found in each sample were in the range 822–957 ng L−1) and unquantifiable to 1368 ng kg−1 (the total concentration of analytes found in each sample were in the range 2251–2992 ng kg−1) in water and sediment, respectively.
研究领域:
环境科学
·
分析化学
·
水质
·
环境监测
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Rui Chang,Xueting Wang,Yanxin Li,Shijuan Zhang
Two pairs of stable isotope labeling (SIL) agents, (4-carboxyphenyl)trimethylammonium iodide (d 0 -CPTA) and its deuterated counterpart d 3 -CPTA, 1-methyl-nicotinamide iodide (d 0 -MNA) and its deuterated counterpart d 3 -MNA, were designed and synthesized. Their mass spectrometry (MS) sensitivity enhancement effect was studied and compared with commercial dansyl chloride to provide inspiration for labeling agent design. CPTA with quaternary ammonium group showed much higher MS sensitivity enhancement effect and was applied to the SIL analysis of alkylamines in food and food packaging materials. The matrix effect was minimized due to the SIL strategy and the permanent charge of the CPTA. The limits of detection (LODs) were in the range of 2.9–5.1 ng/L, and the limits of quantitation (LOQs) were in the range of 9.6–16.8 ng/L. The recoveries ranged from 91.2 % to 97.1 % with relative standard deviations of less than 6.6 %, and the matrix effect ranged from −1.8 % to −4.9 %.
研究领域:
分析化学
·
食品科学
·
质谱
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产品关联
DOI
PubMed
高影响因子
Food Analytical Methods
·
2017
·Vol. 11
·期 3
·790-796
·
IF 2.038
Liang Xu,Feng Ting-Ting,Wu Jian-Hai,Du Ming,Qin Lei,Wang Zhen-Yu,Xu Xian-Bing
Vortex-assisted liquid-liquid micro-extraction (VALLME) was applied for eliminating the matrix effect and improving the sensitivity of eugenol determination by headspace solid phase micro-extraction (HS-SPME) coupled with gas chromatography-mass spectrometer (GC-MS) in fish samples. Under the optimum condition of VALLME and HS-SPME, the good linearity of eugenol in fish samples was obtained in the range from 15.0 to 750.0 μg/kg. The limit of detection (LOD) and the limit of quantification (LOQ) for eugenol were 0.5 and 1.5 μg/kg, respectively. The recovery of eugenol was ranging from 95.4 to 119.9% and the relative standard deviation (RSD %) for eugenol was lower than 20%. The results turned out that VALLME followed HS-SPME-GC-MS was a simple, rapid, and accurate method for the determination of eugenol in fish samples. The levels of eugenol in different parts of real samples were tested by the developed method, and the results concluded that the developed method was compatible with GC-MS analysis with long-term application and had excellent repeatability, linearity, and sensitivity.
研究领域:
分析化学
·
环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Xiao-Kang Fu,Si-Qi Han,Xiao-Bo Zhao,Jing-Yan Kang,Wei Ha,Yan-Ping Shi
Steroid hormone residues in food are a significant sources of endocrine disrupting chemicals (EDCs) that can adversely affect public health. However, the current analytical methods for determining steroid hormones using liquid chromatography-tandem mass spectrometry (LC-MS/MS) can be challenging due to the poor ionization efficiency of steroid hormones and the matrix effect of complex food samples. Herein, based on Cu(I)-catalyzed azide-alkyne cycloaddition (CuAAC) reaction and stable isotope labeling (SIL) technique, a novel pair of chemoselective probes ABI / d 5 -ABI was precisely designed and synthesized. This pair of probes comprises a H/D isotope tag, a linker, a reactive site azido group (N 3 ) and a MS tag (imidazolium salt). The probe ABI was employed to label ethynyl-containing steroid hormones in real samples and d 5 -ABI was applied to label standards, respectively, followed by mixing the two labeled samples for high performance (HP)LC-MS/MS analysis. It was found that the ionization efficiencies of target analytes were increased by 17–4532 folds after ABI labeling. More importantly, the heavy labeled samples serving as internal standards (ISs) can effectively compensate matrix effect during HPLC-MS/MS analysis. Finally, the proposed SIL-HPLC-MS/MS method was successfully used to highly sensitive determine four synthetic steroid hormones in food samples (milk, pork and egg). Furthermore, the good detection limits (0.015–0.020 ng/mL), satisfactory recoveries (75.7–122.9 %), and precisions (RSDs less than 9.2 %) were obtained. Hence, the established method not only provides new insights in designing SIL probes for determination of ethynyl-containing analytes within complex matrix, but also extends the application of CuAAC reaction in the field of food chemistry.
研究领域:
分析化学
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食品科学
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质谱技术
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产品关联
DOI
高影响因子
NORDIC PULP & PAPER RESEARCH JOURNAL
·
2019
·Vol. 34
·期 3
·326-333
·
IF 0.929
Qi Wei,Hao Cheng,Shubin Wu,Chunxia Chen
A convenient and quick method has been developed for simultaneous detection of several low molecular weight chlorinated organic compounds (LMWC) in polyamideamine-epichlorohydrin (PAE) solution, using headspace-solid phase microextraction-gas chromatography (HS-SPME-GC). The method consists of extracting a sample containing 0.42 g/mL NaCl with an 85 µm polyacrylate (PA) coated fiber at an extraction temperature of 45 ∘ C , for an extraction time of 30 mins, and desorbing the analytes at 240 ∘ C for 6 mins. Under these optimized conditions, relatively low limits of detection (LOD) of the analytes, good linearity ( r 2 ≥ 0.9934 ) and precision (relative standard deviation ( RSD ≤ 4.38 % )) were obtained. Taking into account the matrix effect, standard addition methodology was applied to validate this method and recovery values were between 91.59 % and 109.69 %. This method is therefore well-suited for accurate determination of low levels of LMWC in PAE.
研究领域:
分析化学
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环境科学
·
化工工程
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Ying-Ying Jin,Zi-Qi Shi,Wen-Qi Chang,Lin-Xiu Guo,Jian-Liang Zhou,Jian-Qun Liu,Li-Fang Liu,Gui-Zhong Xin
Recent studies have demonstrated the important role of short-chain fatty acids (SCFAs) in the maintenance of homeostasis of respiratory immunity. However, there is still no report focus on the determination of SCFAs level in bronchoalveolar lavage fluid (BALF), the most common sample used for screening biomarkers of the pulmonary diseases. Herein, an ultra-high-performance liquid chromatography with LTQ-Orbitrap mass spectrometer (UHPLC-LTQ-Orbitrap) oriented 3-nitrophenylhydrazine (3-NPH)-based derivatization method was developed for the quantification of SCFAs in BALF. To achieve accurate quantitation, d4-acetate was used as internal standard to compensate for the matrix effects. Method validation showed a good linearity ( R 2 > 0.9992) with wide concentration range, and the intra-day and inter-day precision for determination of eight SCFAs in BALF samples was ≤ 14.79%. The quantitation accuracy, assessed by relative recoveries, ranged from 90% to 110% for target SCFAs at three concentration levels. Matrix effects ranged from 85% to 115%, and the lower limits of quantification of these targeted SCFAs were varied from 3 to 24 nmol/L. The SCFAs-targeted method was then applied to determine the changed levels in BALF samples from OVA-induced asthma mice and normal mice. In addition, the universality of our developed method was also demonstrated by determining the SCFAs concentrations in feces, serum and lung tissue samples from asthma and normal mice. These results indicate that 3-NPH derivatization based UHPLC-LTQ-Orbitrap provides accurate view of global SCFAs alternation in different samples, giving a support to deduce the origin of SCFAs in lung. The present study is of great importance for understanding the role of SCFAs in modulation of host metabolism and immunity.
研究领域:
分析化学
·
呼吸医学
·
免疫学
·
质谱技术
✓ 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）