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Use of Design of Experiments to Optimize the Chromatographic Separation and Ultrasound-Assisted Extraction for Simultaneous Determination of Methylxanthines and Flavonoids in Guarana 利用实验设计优化色谱分离和超声辅助萃取法同时测定瓜拉纳中的甲基黄嘌呤和黄酮类化合物
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-19 DOI: 10.1007/s12161-024-02618-5
Pedro Kaynnan C. Barreto, André Luiz S. da Silva Jr., Robson M. de Jesus, Janclei P. Coutinho, Ivon P. Lôbo, Herick M. Santos, Raildo Mota de Jesus

In this work, Design of Experiments and the Derringer’s desirability function were used to optimize the chromatographic conditions and an ultrasound-extraction procedure for the simultaneous determination of caffeine, theobromine, theophylline, catechin, and epicatechin in guarana seeds by HPLC-UV/Vis. The composition of the mobile phase was optimized using a mixture design, where an adequate chromatographic separation was obtained with 92.4% of an aqueous solution of acetic acid (0.1% v v− 1), 5.2% methanol, and 2.4% isopropanol. A mixture design using water, acetone, and ethanol was used to optimize the composition of the extractor solution for ultrasound-assisted extraction. The best conditions for simultaneous extraction of the target compounds were 1.45, 0.45, and 0.1 mL of water, ethanol, and acetone, respectively. After defining the extractor solution, we applied a Doehlert matrix to study the instrumental conditions of the ultrasonic bath. Instrumental parameters were optimized at 35 °C, 30% and 10.5 min for temperature, power, and extraction time, respectively. The proposed procedure was validated and applied for analysis of guarana seeds samples dried by different techniques. Our results indicated that post-harvest management can significantly change the catechin and epicatechin contents in guarana samples.

本研究采用实验设计和德林格尔期望函数优化色谱条件和超声萃取程序,以 HPLC-UV/Vis 法同时测定瓜拉纳种子中的咖啡因、可可碱、茶碱、儿茶素和表儿茶素。采用混合设计优化了流动相的组成,其中 92.4% 的醋酸水溶液(0.1% v v-1)、5.2% 甲醇和 2.4% 异丙醇可获得充分的色谱分离。水、丙酮和乙醇的混合设计用于优化超声辅助萃取的萃取液成分。同时萃取目标化合物的最佳条件分别为 1.45、0.45 和 0.1 mL 水、乙醇和丙酮。确定萃取溶液后,我们采用多赫勒特矩阵来研究超声波浴的仪器条件。对仪器参数进行了优化,温度、功率和萃取时间分别为 35°C、30% 和 10.5 分钟。所提出的程序得到了验证,并被用于分析用不同技术干燥的瓜拉纳种子样品。结果表明,收获后的管理会显著改变瓜拉纳种子样品中儿茶素和表儿茶素的含量。
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引用次数: 0
Optimization of Process Parameters Using Response Surface Methodology for Essential Oil Extraction from Canarium odontophyllum Kernels by Subcritical Water Treatment 利用响应面方法优化亚临界水处理法从大叶女贞果仁中提取精油的工艺参数
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-19 DOI: 10.1007/s12161-024-02624-7
Muhammad Hazwan Hamzah, Nurbalqis Zulkefli, Adila Fazliyana Aili Hamzah, Rosnah Shamsudin, Hasfalina Che Man, Abd Halim Md Ali, Maimunah Mohd Ali, Bernard Maringgal, Mohd Hafizz Wondi

The physicochemical properties of dabai kernel oil as well as the morphology of dabai samples are affected by the optimal extraction method and process configurations. Subcritical water treatment prior to dabai kernel oil extraction was optimized through the utilization of response surface methodology based on central composite design. The subcritical water treatment was carried out within the following temperature ranges of 100 to 150 °C, 10- to 20-min reaction times, and 10:1 to 20:1 solvent to solid ratios. Results showed that temperature of 100 °C, reaction time of 10 min, and solvent to solid ratio of 10:1 were optimal parameters for dabai kernel oil by subcritical water treatment prior to Soxhlet extraction. Dabai kernel oil yields via subcritical water treatment were 96.53% on average, compared to 42.85% for Soxhlet extraction sample. Gas chromatography mass spectrometry analysis found for subcritical water treatment samples revealed value-added compounds, including oxalic acid and 9-octadecenoic acid, which can be utilized for cleaning and pharmaceutical applications. Scanning electron microscope images provided evidence that rapid extraction was driven by the degradation and aggregation of dabai kernel powder structure. The Brunauer–Emmett–Teller analysis indicated that the dabai kernel of subcritical water treatment displayed a greater surface area (14.813 m2/g) than the raw (2.804 m2/g) or Soxhlet extraction (13.452 m2/g) dabai kernel. Subcritical water treatment could be considered a promising method in combination with Soxhlet extraction in order to improve the oil yield from dabai kernels.

达巴依仁油的理化性质以及达巴依样品的形态会受到最佳提取方法和工艺配置的影响。通过利用基于中心复合设计的响应面方法,对提取达巴依仁油之前的亚临界水处理进行了优化。亚临界水处理的温度范围为 100 至 150 °C,反应时间为 10 至 20 分钟,溶剂与固体的比例为 10:1 至 20:1。结果表明,温度为 100 °C、反应时间为 10 分钟、溶剂与固体的比例为 10:1 是在索氏提取之前用亚临界水处理达巴依仁油的最佳参数。经亚临界水处理的达拜仁油平均产率为 96.53%,而索氏提取样品的平均产率为 42.85%。对亚临界水处理样品进行的气相色谱质谱分析发现了增值化合物,包括草酸和 9-十八烯酸,可用于清洁和制药。扫描电子显微镜图像证明,快速萃取是由达贝仁粉末结构的降解和聚集驱动的。布鲁瑙尔-埃美特-泰勒分析表明,经亚临界水处理的大白果仁的比表面积(14.813 平方米/克)大于未加工的大白果仁(2.804 平方米/克)或索氏提取的大白果仁(13.452 平方米/克)。亚临界水处理与索氏提取相结合,可被视为提高大白果仁出油率的一种有前途的方法。
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引用次数: 0
Evaluation of Total Phenolic, Flavonoid Contents, and Antioxidant Activities of Seed Extracted from Coriander (Coriandrum sativum L.) and Black Cumin (Nigella sativa) Spices 芫荽(Coriandrum sativum L.)和黑小茴香(Nigella sativa)香料籽提取物的总酚类、类黄酮含量和抗氧化活性评估
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-19 DOI: 10.1007/s12161-024-02622-9
Dessie Tibebe, Abebaw Belete, Yezbie Kassa, Marye Mulugeta, Zerubabel Moges, Dereje Yenealem, Tarekegn Fentie, Agmas Amare

Black cumin (Nigella sativa) and coriander (Coriandrum sativum L.) are common culinary spices that are used singly or combined in the diet of many populations of Ethiopia, and there is a long-held belief of their health-enhancing properties. The present study was designed to investigate the antioxidant properties, phenolic and flavonoid contents of aqueous methanolic extracts from Nigella sativa and Coriandrum sativum L. seed samples. The contents of polyphenols and flavonoids were evaluated by colorimetric method, and antioxidant activity was determined based on the ability to scavenge free radicals by using DPPH assay. An aqueous methanol extract of Coriandrum sativum L. resulted in the highest phenolic content from West Dembia (1.799 ± 0.0011 mg GAE/g), followed by Nigella sativa from East and West Dembia (1.737 ± 0.0014 & 1.734 ± 0.0013 mg gallic acid equivalent per gram (mg GAE/g) respectively) and Coriandrum sativum L. from West Dembia (1.678 ± 0.0018 mg GAE/g) measured by the Folin–Ciocalteu reagent method. The greatest flavonoid content was observed with extracts of Coriandrum sativum L. (1.114 ± 0.0005 mg quercetin equivalents per gram samples (mg QE/g)) from East Dembia district followed by Nigella sativa (1.002 ± 0.0007 (mg QE/g)) as measured by an aluminum chloride colorimetric method, while the least was recorded for Coriandrum sativum L. (0.926 ± 0.0013 mg QE/g) and Nigella sativa (0.764 ± 0.0010 mg QE/g) from West Dembia district. Among the two selected spice extracts, Nigella sativa from East Dembia district displayed the highest DPPH radical scavenging activity with an IC50 value 432-mg ascorbic acid equivalent per gram sample (AAE/g), while Nigella sativa and Coriandrum sativum L. from West Dembia and Coriandrum sativum L. (East Dembia) showed lower antioxidant activities having 372, 320, and 366 mg AAE/g of sample respectively. These results confirmed that Nigella sativa and Coriandrum sativum L. extracts possess appreciable natural antioxidant potentials, thereby providing good justification for their increased domestication and combined food consumption.

黑孜然(Nigella sativa)和芫荽(Coriandrum sativum L.)是常见的烹饪香料,埃塞俄比亚的许多居民在饮食中单独或混合使用这些香料,人们长期以来一直认为它们具有增进健康的功效。本研究旨在调查 Nigella sativa 和 Coriandrum sativum L. 种子样品水甲醇提取物的抗氧化特性、酚类和类黄酮含量。多酚和类黄酮的含量采用比色法进行评估,抗氧化活性则根据清除自由基的能力采用 DPPH 法进行测定。西登比亚的芫荽甲醇水提取物酚含量最高(1.799 ± 0.0011 毫克 GAE/克),其次是东登比亚和西登比亚的黑麦草(1.737 ± 0.0014 毫克 GAE/克和 1.737 ± 0.0011 毫克 GAE/克)。0014 & 1.734 ± 0.0013 毫克没食子酸当量(mg GAE/g))和西登比亚的芫荽(1.678 ± 0.0018 毫克 GAE/g)。黄酮含量最高的是东登比亚地区的芫荽提取物(1.114 ± 0.0005 毫克槲皮素当量/克样品(mg QE/g)),其次是黑麦草提取物(1.002 ± 0.0007 毫克槲皮素当量/克样品(mg QE/g))。通过氯化铝比色法测量,东登比亚地区的芫荽(0.926 ± 0.0013 毫克槲皮素当量/克)和西登比亚地区的黑麦草(0.764 ± 0.0010 毫克槲皮素当量/克)的槲皮素含量最低。在所选的两种香料提取物中,东登比亚地区的黑奴属植物显示出最高的 DPPH 自由基清除活性,IC50 值为每克样品 432 毫克抗坏血酸当量(AAE/g),而西登比亚地区的黑奴属植物和芫荽属植物以及东登比亚地区的芫荽属植物则显示出较低的抗氧化活性,分别为每克样品 372、320 和 366 毫克 AAE/g。这些结果证实,Nigella sativa 和 Coriandrum sativum L. 提取物具有可观的天然抗氧化潜力,从而为它们的驯化和综合食用提供了充分的理由。
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引用次数: 0
Authenticity Determination of Goat Cheese In Mexico Using qPCR Assay 利用 qPCR 检测法确定墨西哥山羊奶酪的真伪
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-17 DOI: 10.1007/s12161-024-02617-6
Jesús Daniel Villanueva-Zayas, Roberto Rodríguez-Ramírez, Alma Guadalupe Villa-Lerma, Luz Angélica Ávila-Villa, Marco Antonio Ceballos-Fabela, Juan Francisco Hernández-Chávez, Alejandro Miguel Figueroa-López

In recent years, the Mexican government has implemented several economic sanctions on producers and marketers of milk bovine cheese due to food fraud such as mislabeling or addition of vegetable fats. However, there have been no official reports on the authenticity of goat cheese. This research aimed to detect adulteration in goat cheese by terms of food substitution with bovine milk or soy protein. For which, bovine cytochrome b genes (274 bp) and lectin genes (118 bp) were amplified in 12 commercial brands of goat cheese by real-time PCR (qPCR) where the detection limit for each species was assigned to the lowest concentration detected with a confidence level ≥ 95% being 0.01 ng/µL for bovine milk, and 0.1 ng/µL for soy DNA. Research findings indicate the absence of soy protein; however, a high degree of adulteration with bovine milk (92.3%) was found. The above evidence suggests the need for regulatory agencies to improve verification and traceability mechanisms to ensure the authenticity of these products and protect consumers by providing reliable information.

近年来,由于食品欺诈(如贴错标签或添加植物脂肪),墨西哥政府对牛奶牛奶酪的生产商和销售商实施了多次经济制裁。然而,还没有关于山羊奶酪真伪的官方报告。这项研究旨在通过用牛乳或大豆蛋白替代食品来检测山羊奶酪的掺假情况。为此,研究人员通过实时 PCR(qPCR)技术,对 12 个品牌的山羊奶酪中的牛细胞色素 b 基因(274 bp)和凝集素基因(118 bp)进行了扩增,每个物种的检测限为检测到的最低浓度,置信度≥95%,牛乳为 0.01 ng/µL,大豆 DNA 为 0.1 ng/µL。研究结果表明不含大豆蛋白,但发现牛乳的掺假程度很高(92.3%)。上述证据表明,监管机构有必要改进验证和溯源机制,以确保这些产品的真实性,并通过提供可靠的信息来保护消费者。
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引用次数: 0
Identification of Adulterated Cooking Oil by Raman Spectroscopy 利用拉曼光谱鉴别掺假食用油
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-17 DOI: 10.1007/s12161-024-02626-5
Hina Shehnaz, Ayesha Ashraf, Muhammad Irfan Majeed, Haq Nawaz, Maira Afzal, Muhammad Zeeshan Majeed, Muhammad Idrees Jilani, Muhammad Waseem Akram, Rabeea Razaq, Eiman Sultan, Naeema Kanwal, Urwa Shahid

A better quality of life comes with a healthy diet without adulteration or contamination. As much as the demand for purity in diet increases, the risk of adulteration also increases in daily edibles. The present study proposed Raman spectroscopy for the identification of used cooking oils to overcome adulteration. Unused cooking oil with different concentrations of used oil (waste oil) as an adulterant was examined by Raman spectroscopy along with principal component analysis (PCA). Increasing the concentration of used oil causes changes in Raman spectral features. The changes can be observed at 1413 cm−1, 1521 cm−1, and 1745 cm−1 in Raman mean spectra of unused oil with the addition of different concentrations of the adulterant. Raman spectroscopy with PCA gives qualitative analysis and helps to monitor the quality of the cooking oil. PCA is a statistical tool that is used to examine variations in the given Raman spectral dataset. PC-1 shows more variability about 93.8% for the differentiation of the Raman spectral groups of the used and unused oil, while for unused oil and its different concentrations with adulterant, it shows a variability of 88.8%. These results demonstrate that Raman spectroscopy can be applied for the identification of adulterated oil. In the future, this spectroscopic technique can be used in the field of food chemistry because of its non-invasiveness and non-destructive analysis.

没有掺假或污染的健康饮食能带来更好的生活质量。随着人们对饮食纯度的要求越来越高,日常食品中掺假的风险也随之增加。本研究建议使用拉曼光谱鉴别使用过的食用油,以防止掺假。通过拉曼光谱和主成分分析法(PCA)对掺入不同浓度废油的未使用食用油进行了检测。废油浓度的增加会导致拉曼光谱特征发生变化。添加不同浓度的掺杂剂后,未使用过的油的拉曼光谱平均值在 1413 厘米-1、1521 厘米-1 和 1745 厘米-1 处会发生变化。利用 PCA 进行拉曼光谱定性分析,有助于监测食用油的质量。PCA 是一种统计工具,用于研究给定拉曼光谱数据集的变化。PC-1 在区分使用过的油和未使用过的油的拉曼光谱组方面显示出更大的变异性,约为 93.8%,而对于未使用过的油及其不同浓度的掺杂物,则显示出 88.8%的变异性。这些结果表明,拉曼光谱可用于鉴别掺假油。由于这种光谱技术具有非侵入性和非破坏性分析的特点,因此今后可用于食品化学领域。
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引用次数: 0
Correction: Cold-induced Homogenous Liquid–Liquid Extraction Performed in a Refrigerated Centrifuge Combined with Deep Eutectic Solvent-based Dispersive Liquid–Liquid Microextraction for the Extraction of Some Endocrine Disrupting Compounds and Hydroxymethylfurfural from Honey Samples 更正:在冷冻离心机中进行冷诱导均匀液-液萃取,结合基于深共晶溶剂的分散液-液微萃取,从蜂蜜样品中萃取某些干扰内分泌的化合物和羟甲基糠醛
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-17 DOI: 10.1007/s12161-024-02585-x
Fatemeh Khani, J. Khandaghi, Mir Ali Farajzadeh, Mohammad Reza Afshar Mogaddam
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引用次数: 0
Enhanced Antenna System for Non-invasive Quality Assessment and Defect Identification in Fruits: Uniting Tomographic Image Reconstruction with FTIR Spectroscopy 用于水果无创质量评估和缺陷识别的增强型天线系统:将断层图像重建与傅立叶变换红外光谱技术相结合
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-15 DOI: 10.1007/s12161-024-02621-w
Md. Najumunnisa, A. S. C. S. Sastry, B. T. P. Madhav, Ahmed Nabih Zaki Rashed

This study presents a comprehensive exploration of an antenna system designed for tomographic image reconstruction, with a particular focus on the application to various fruits. The antenna, simulated using CST software and physically manufactured, operates in two frequency bands (0.915 GHz and 2.45 GHz) and is arranged in a circular configuration for signal reception. The experimental setup incorporates a microwave source generator, an 8-element antenna array, a vector network analyzer (VNA), and probes. Employing the “Dielectric Anomaly Detection Approach,” the system achieves detailed tomographic reconstructions, emphasizing dielectric anomalies in defective fruit regions. Additionally, Fourier transform infrared (FTIR) spectroscopy is employed to examine the molecular composition of fruit specimens, providing insights into their chemical properties. The non-invasive nature of the experimental setup is highlighted in contrast to the invasive FTIR method, offering advantages in assessing fruit quality without altering specimens.

本研究全面探讨了为断层扫描图像重建而设计的天线系统,尤其侧重于各种水果的应用。该天线使用 CST 软件模拟并实际制造,工作在两个频段(0.915 GHz 和 2.45 GHz),以圆形配置接收信号。实验装置包括微波源发生器、8 元天线阵列、矢量网络分析仪(VNA)和探头。该系统采用 "介电异常检测方法",实现了详细的层析成像重建,强调了有缺陷果实区域的介电异常。此外,还采用傅立叶变换红外(FTIR)光谱来检测水果样本的分子组成,从而深入了解其化学特性。与侵入式傅立叶变换红外光谱法相比,该实验装置具有非侵入性特点,在评估水果质量时无需改变标本。
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引用次数: 0
Utilization of a Resonant Cavity for Characterization of Single In-Shell Peanuts 利用谐振腔表征单粒带壳花生
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-13 DOI: 10.1007/s12161-024-02620-x
M. A. Lewis, S. Trabelsi, R. S. Bennett, K. D. Chamberlin

Peanuts are taken through routine postharvest procedures to assess quality, establish the grade, and determine the amount of revenue that the farmer will be allotted. Moisture content and meat content are examples of parameters determined to assess the grade of the peanuts. Such parameters are assessed for bulk samples usually with mass > 1 kg, and the resulting values are averages of peanuts within the bulk sample. Such processes are destructive and lack provision for assessment of single, in-shell peanuts. Thus, the characterization of single, in-shell peanuts was investigated by measuring the shift in resonant frequency and the change in cavity transmission characteristics caused by each peanut once inserted into a resonant cavity connected to a vector network analyzer (VNA). Such microwave measurements were taken for over 300 in-shell peanuts at 22 °C. The peanuts were divided into seven categories based on custom fillings to simulate diseased and damaged peanuts. One category, serving as the control, consisted of intact peanuts, while the other categories consisted of peanuts filled with coffee, cornstarch, and/or a single kernel. The measured resonant-cavity parameters and the calculated dielectric properties provided a means to characterize each in-shell peanut. Statistical analysis was performed to assess differentiation between the seven categories using those parameters. Kruskal–Wallis One-Way ANOVA on Ranks, Tukey test, and Dunn’s Method were used to determine which categories were statistically significantly different from each other for each parameter at the 95% confidence interval. Lastly, artificial intelligence was used to investigate the creation of models to accurately classify the peanuts.

花生收获后要经过例行程序,以评估质量,确定等级,并确定农民的收入额。水分含量和肉含量是评估花生等级的参数。这些参数是对质量通常为 1 千克的散装样本进行评估,得出的数值是散装样本中花生的平均值。这种方法具有破坏性,而且无法对单个带壳花生进行评估。因此,通过测量每粒花生在插入与矢量网络分析仪(VNA)相连的谐振腔后引起的谐振频率偏移和腔体传输特性的变化,对单粒带壳花生的特性进行了研究。这种微波测量是在 22 °C 下对 300 多颗带壳花生进行的。这些花生根据定制的填充物被分为七类,以模拟患病和受损的花生。其中一类作为对照,由完整的花生组成,而其他类别则由填充了咖啡、玉米淀粉和/或单一果仁的花生组成。通过测量谐振腔参数和计算介电特性,可以确定每种壳内花生的特征。使用这些参数进行了统计分析,以评估七个类别之间的差异。使用 Kruskal-Wallis 单向方差分析、Tukey 检验和 Dunn 方法来确定在 95% 的置信区间内,哪些类别的每个参数在统计上有显著差异。最后,研究人员利用人工智能建立模型,对花生进行准确分类。
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引用次数: 0
Selective and Rapid Detection of Minocycline in Milk Using a Novel Fluorescence Conjugated Polymer Probe 利用新型荧光共轭聚合物探针选择性快速检测牛奶中的米诺环素
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-04-13 DOI: 10.1007/s12161-024-02619-4
Lindan Gong, Lin Zhang, Hengyuan Wang, Yan Sun, Hongju Zhang, Lu-an Fan

Minocycline is a broad-spectrum antibiotic widely used in clinical and veterinary medicine and its adverse effects are as prominent as its potent efficacy. To avoid its abuse and accumulation, it is very important to detect minocycline in medical science, food industry, and aquaculture industry. Here, a conjugated polymer probe for minocycline is prepared and its optical properties and fluorescence response to minocycline is studied. The quenching efficiency is linear relevant with the amount of minocycline at the concentration range of 0–12 µM in PBS and 0–28 µM in ethanol with the limit of detection of 0.0151 µM. Moreover, the standard addition recoveries of minocycline in skim milk samples are between 92.22 and 104.43%, and the relative standard deviation values are less than 3%. These results imply that the probe has a great potential for detecting minocycline in actual samples with simplify, rapidity, and sensitivity.

米诺环素是一种广谱抗生素,广泛应用于临床和兽医领域,其不良反应与强大的药效同样突出。为避免其滥用和蓄积,在医学、食品工业和水产养殖业中检测米诺环素非常重要。本文制备了一种米诺环素共轭聚合物探针,并研究了其光学性质和对米诺环素的荧光响应。在 PBS 中 0-12 µM 和乙醇中 0-28 µM 的浓度范围内,淬灭效率与米诺环素的量呈线性关系,检测限为 0.0151 µM。此外,脱脂奶样品中米诺环素的标准添加回收率在 92.22% 至 104.43% 之间,相对标准偏差值小于 3%。这些结果表明,该探针在检测实际样品中的米诺环素方面具有很大的潜力,而且简单、快速、灵敏。
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引用次数: 0
Multi-plug Filtration Purification Combined with High-Performance Liquid Chromatography-Tandem Mass Spectrometry for the Simultaneous Determination of Pesticides, Veterinary Drugs, Mycotoxins, and Persistent Organic Pollutants in Livestock and Poultry Meat 多孔过滤净化结合高效液相色谱-串联质谱法同时测定畜禽肉中的农药、兽药、霉菌毒素和持久性有机污染物
IF 2.6 3区 农林科学 Q2 FOOD SCIENCE & TECHNOLOGY Pub Date : 2024-03-26 DOI: 10.1007/s12161-024-02615-8
Xuwei Guo, Youzhi Su, Jun Liu, Yanmei Li, Fang Li, Hongqin Lei

A method for the determination of 106 pesticides, 74 veterinary drugs, 10 mycotoxins, and 18 persistent organic pollutants in livestock and poultry meat was developed and validated in the present study. The meat was extracted with acetonitrile under citric acid caching and purified using the multi-plug filtration clean-up (m-PFC) column. The components were separated using liquid chromatography on a C18 column and then eluted using a gradient of the aqueous solutions of acetonitrile and 0.1% formic acid (containing 2 mmol/L ammonium acetate) as the mobile phase. The mass spectrometry analysis was performed next using two electrospraying scan modes—the positive ion mode and the negative ion mode, and multiple reaction monitoring (MRM) modes. The results revealed that all 208 target analytes exhibited good linearity in their respective linear ranges, with the correlation coefficient of each analyte above 0.9953 and the corresponding limits of quantification (LOQs) in the range of 0.1–9.8 µg/kg. The average recovery values of 189 targets at three different spiked levels of low, medium, and high ranged from 70.1 to 120.0%, and the corresponding values of relative standard deviation (RSD) ranged from 1.3 to 15.0%, respectively. The remaining 19 targets exhibited the average recovery values [at three different spiked levels of low, medium, and high] ranging from 18.6 to 58.9%, with the corresponding RSD values ranging from 1.5 to 11.3%. The developed method was applied to 132 batches of livestock and poultry meat, and nine pesticides and seven veterinary drugs were detected in the concentration range of 0.1–24.8 µg/kg. These results suggested that the developed method is simple, reliable, reproducible, and suitable for the determination of pesticides, veterinary drugs, mycotoxins, and persistent organic pollutants in livestock and poultry meat.

本研究建立并验证了测定畜禽肉中106种农药、74种兽药、10种霉菌毒素和18种持久性有机污染物的方法。畜禽肉在柠檬酸缓蚀条件下用乙腈提取,然后用多管柱过滤净化(m-PFC)柱净化。采用 C18 色谱柱进行液相色谱分离,然后以乙腈和 0.1% 甲酸水溶液(含 2 mmol/L 乙酸铵)的梯度洗脱作为流动相。接下来使用两种电喷雾扫描模式--正离子模式和负离子模式以及多反应监测(MRM)模式进行了质谱分析。结果表明,所有 208 种目标分析物在各自的线性范围内均表现出良好的线性关系,每种分析物的相关系数均高于 0.9953,相应的定量限(LOQ)范围为 0.1-9.8 µg/kg。189 个目标物在低、中、高三种不同加标水平下的平均回收率为 70.1% 至 120.0%,相对标准偏差(RSD)分别为 1.3% 至 15.0%。其余 19 个目标物在低、中、高三种不同加标水平下的平均回收率为 18.6% 至 58.9%,相应的 RSD 值为 1.5% 至 11.3%。对 132 批畜禽肉进行了检测,在 0.1-24.8 µg/kg 的浓度范围内检出了 9 种农药和 7 种兽药。结果表明该方法简便、可靠、重现性好,适用于畜禽肉中农药、兽药、霉菌毒素和持久性有机污染物的检测。
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Food Analytical Methods
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