Junmei Ma, Qiang Li, Yonghuan Yan, Lei Sun, Pin Lv, Yan Zhang
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In this study, we have established a workflow for the rapid screening and confirmation of four cholinomimetics in edible fungi and areca nut by using the QuEChERS pretreatment method and ultra-high performance liquid chromatography coupled with quadrupole/time-of-flight mass spectrometry (UPLC-Q-TOF/MS) for the first time.</p><p><b>Methods:</b> The samples were extracted with acetonitrile, and separation was achieved on a HILIC column (2.1 mm × 100 mm, 1.6 μm) with acetonitrile and 20 mM ammonium formate aqueous solution as mobile phase with gradient elution. UPLC-Triple TOF™6600<sup>+</sup> was used to collect the data of the target analytes in the mode of TOF-MS-IDA-MS/MS, and the data were analyzed by SCIEX OS software to realize the qualitative screening and confirmation of samples.</p><p><b>Results:</b> The mass accuracy error of 4 cholinomimetics was lower than 5.0 × 10<sup>−6</sup>. All four cholinomimetic compounds had good linearity in a certain range, and the correlation coefficient (<i>R</i><sup>2</sup>) was higher than 0.998. The limits of detection and limits of quantification of the method were 2.5–25.0 μg/kg and 5.0–50.0 μg/kg, respectively. The recoveries were between 81.0% and 99.1% at spiked level 5.0–500.0 μg/kg, with the relative standard deviation of 0.41%–4.00%.</p><p><b>Conclusion:</b> The method is sensitive, accurate, and suitable for rapid screening and confirmation of 4 cholinomimetics in edible fungi and areca nut.</p>","PeriodicalId":15951,"journal":{"name":"Journal of Food Quality","volume":"2025 1","pages":""},"PeriodicalIF":2.9000,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1155/jfq/7038821","citationCount":"0","resultStr":"{\"title\":\"Determination of Four Cholinomimetics in Edible Fungi and Areca Nut Using Ultra-High Performance Liquid Chromatography Combined With Quadrupole/Time-of-Flight Mass Spectrometry\",\"authors\":\"Junmei Ma, Qiang Li, Yonghuan Yan, Lei Sun, Pin Lv, Yan Zhang\",\"doi\":\"10.1155/jfq/7038821\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><b>Background:</b> Cholinomimetic compounds are a class of organic compounds found in natural plants that have significant biological activity as well as toxicity, and their dosage must be controlled, with side effects occurring in case of accidental ingestion or excessive intake. Accurate determination of four cholinomimetic compounds in edible fungi and areca nut can provide technical support to the relevant monitoring organizations, which is conducive to the protection of consumer health. In this study, we have established a workflow for the rapid screening and confirmation of four cholinomimetics in edible fungi and areca nut by using the QuEChERS pretreatment method and ultra-high performance liquid chromatography coupled with quadrupole/time-of-flight mass spectrometry (UPLC-Q-TOF/MS) for the first time.</p><p><b>Methods:</b> The samples were extracted with acetonitrile, and separation was achieved on a HILIC column (2.1 mm × 100 mm, 1.6 μm) with acetonitrile and 20 mM ammonium formate aqueous solution as mobile phase with gradient elution. UPLC-Triple TOF™6600<sup>+</sup> was used to collect the data of the target analytes in the mode of TOF-MS-IDA-MS/MS, and the data were analyzed by SCIEX OS software to realize the qualitative screening and confirmation of samples.</p><p><b>Results:</b> The mass accuracy error of 4 cholinomimetics was lower than 5.0 × 10<sup>−6</sup>. All four cholinomimetic compounds had good linearity in a certain range, and the correlation coefficient (<i>R</i><sup>2</sup>) was higher than 0.998. The limits of detection and limits of quantification of the method were 2.5–25.0 μg/kg and 5.0–50.0 μg/kg, respectively. 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引用次数: 0
摘要
背景:拟胆碱化合物是一类天然植物中发现的具有显著生物活性和毒性的有机化合物,其剂量必须控制,误食或过量摄入会产生副作用。准确测定食用菌和槟榔中4种类胆碱化合物,可为相关监测机构提供技术支持,有利于保护消费者健康。本研究首次采用QuEChERS预处理方法和超高效液相色谱-四极杆/飞行时间质谱联用(UPLC-Q-TOF/MS)技术,建立了食用菌和槟榔中4种胆碱模拟物的快速筛选和鉴定流程。方法:用乙腈提取样品,以乙腈和20 mm甲酸铵水溶液为流动相,采用梯度洗脱,采用HILIC柱(2.1 mm × 100 mm, 1.6 μm)分离。采用UPLC-Triple TOF™6600+,以TOF-MS- ida -MS/MS模式采集目标分析物数据,采用SCIEX OS软件对数据进行分析,实现样品的定性筛选和确认。结果:4种仿胆碱制剂的质量精度误差均小于5.0 × 10−6。4种拟胆碱类化合物在一定范围内线性良好,相关系数(R2)均大于0.998。方法的检出限为2.5 ~ 25.0 μg/kg,定量限为5.0 ~ 50.0 μg/kg。加标水平为5.0 ~ 500.0 μg/kg时,加标回收率为81.0% ~ 99.1%,相对标准偏差为0.41% ~ 4.00%。结论:该方法灵敏、准确,适用于食用菌和槟榔中4种拟胆碱物质的快速筛选和确证。
Determination of Four Cholinomimetics in Edible Fungi and Areca Nut Using Ultra-High Performance Liquid Chromatography Combined With Quadrupole/Time-of-Flight Mass Spectrometry
Background: Cholinomimetic compounds are a class of organic compounds found in natural plants that have significant biological activity as well as toxicity, and their dosage must be controlled, with side effects occurring in case of accidental ingestion or excessive intake. Accurate determination of four cholinomimetic compounds in edible fungi and areca nut can provide technical support to the relevant monitoring organizations, which is conducive to the protection of consumer health. In this study, we have established a workflow for the rapid screening and confirmation of four cholinomimetics in edible fungi and areca nut by using the QuEChERS pretreatment method and ultra-high performance liquid chromatography coupled with quadrupole/time-of-flight mass spectrometry (UPLC-Q-TOF/MS) for the first time.
Methods: The samples were extracted with acetonitrile, and separation was achieved on a HILIC column (2.1 mm × 100 mm, 1.6 μm) with acetonitrile and 20 mM ammonium formate aqueous solution as mobile phase with gradient elution. UPLC-Triple TOF™6600+ was used to collect the data of the target analytes in the mode of TOF-MS-IDA-MS/MS, and the data were analyzed by SCIEX OS software to realize the qualitative screening and confirmation of samples.
Results: The mass accuracy error of 4 cholinomimetics was lower than 5.0 × 10−6. All four cholinomimetic compounds had good linearity in a certain range, and the correlation coefficient (R2) was higher than 0.998. The limits of detection and limits of quantification of the method were 2.5–25.0 μg/kg and 5.0–50.0 μg/kg, respectively. The recoveries were between 81.0% and 99.1% at spiked level 5.0–500.0 μg/kg, with the relative standard deviation of 0.41%–4.00%.
Conclusion: The method is sensitive, accurate, and suitable for rapid screening and confirmation of 4 cholinomimetics in edible fungi and areca nut.
期刊介绍:
Journal of Food Quality is a peer-reviewed, Open Access journal that publishes original research articles as well as review articles related to all aspects of food quality characteristics acceptable to consumers. The journal aims to provide a valuable resource for food scientists, nutritionists, food producers, the public health sector, and governmental and non-governmental agencies with an interest in food quality.