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用于测定葡萄酒澄清剂PVPP和PVI-PVP聚合物单体的液相色谱-高分辨质谱法的开发与验证

Development and validation of an LC-HRMS method for the determination of monomers of wine fining PVPP and PVI-PVP polymers.

作者信息

Borghini Francesca, Ferrari Stefano, Cavaglioni Alessandro, Consumi Marco, Tamasi Gabriella, Guidugli Federico

机构信息

Department of Biotechnology, Chemistry and Pharmacy, University of Siena, Via Aldo Moro 2, 53100 Siena, Italy; ISVEA, Istituto per Lo Sviluppo Viticolo Enologico ed Agroindustriale, Via Basilicata 1-5, Località Fosci, 53036 Poggibonsi Siena, Italy; Santa Chiara Lab, University of Siena, Via Valdimontone 1, 53100 Siena, Italy.

ISVEA, Istituto per Lo Sviluppo Viticolo Enologico ed Agroindustriale, Via Basilicata 1-5, Località Fosci, 53036 Poggibonsi Siena, Italy.

出版信息

Food Chem. 2025 Nov 1;491:145266. doi: 10.1016/j.foodchem.2025.145266. Epub 2025 Jun 21.

DOI:10.1016/j.foodchem.2025.145266
PMID:40570519
Abstract

A HPLC-HRMS method was developed and validated to analyze the polyvinylimidazole/polyvinylpyrrolidone (PVI/PVP) monomers (N-vinylimidazole, N-vinyl-2-pyrrolidone, imidazole, and 2-pyrrolidone) in wines. The use of a C30 column and HRMS allowed to obtain high selectivity, excluding several interferents. The lower limit of quantification was 10 ng/mL for the targeted molecules and the method was linear from 10 to 1000 ng/mL. Matrix effect (ME) was detected for all compounds, except for N-vinylimidazole and a correction function to overcame ME was suggested with the use of a calibration curve in hydroalcoholic solution. Migration tests demonstrated that imidazole reveals the oenological use of PVI-based products, whereas 2-pyrrolidone represents a very questionable marker for PVPP fining agents since all analyzed wines showed levels of this compound higher than the limit defined by OIV. Further investigations are necessary to test commercial products using both model and real wines in order to find new markers of PVPP treatment.

摘要

开发并验证了一种高效液相色谱-高分辨质谱(HPLC-HRMS)方法,用于分析葡萄酒中的聚乙烯咪唑/聚乙烯吡咯烷酮(PVI/PVP)单体(N-乙烯基咪唑、N-乙烯基-2-吡咯烷酮、咪唑和2-吡咯烷酮)。使用C30柱和高分辨质谱可获得高选择性,排除了多种干扰物。目标分子的定量下限为10 ng/mL,该方法在10至1000 ng/mL范围内呈线性。除N-乙烯基咪唑外,所有化合物均检测到基质效应(ME),建议使用水醇溶液中的校准曲线来克服基质效应的校正函数。迁移试验表明,咪唑揭示了基于PVI产品的酿酒用途,而2-吡咯烷酮对于PVPP澄清剂来说是一个非常可疑的标志物,因为所有分析的葡萄酒中该化合物的含量均高于国际葡萄与葡萄酒组织(OIV)规定的限值。有必要进一步开展研究,使用模型葡萄酒和实际葡萄酒对商业产品进行测试,以找到PVPP处理的新标志物。

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