Critical comparison of the on‐line and off‐line molecularly imprinted solid‐phase extraction of patulin coupled with liquid chromatography

Abstract

Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail.

Mycotoxins-Imprinted Polymers: A State-of-the-Art Review

“…Valve in position A; mycotoxin clean-up and preconcentration. Valve in position B: mycotoxin separation on analytical HPLC column [ 99 ].…”

Solid‐phase extraction techniques based on nanomaterials for mycotoxin analysis: An overview for food and agricultural products

“…As another alternative to IAC, molecular imprinting polymer (MIP) columns have been developed based on molecular recognition mechanism [52]. MIP columns have been commercially available for the analysis of mycotoxins, such as OTA, PAT, and ZEN, due to the advantages of easy preparation, good stability, large specific surface area (SSA), and rich binding sites [64][65][66]. With marketed MIP columns, simultaneous extraction can also be realized for fumonisins/ZEN or aflatoxins/fumonisins/DON/OTA/ZEN/HT-2/T-2.…”

“…It is encouraging that MIPs have been used in online SPE, with nanomaterial-based SPE as the first dimension for sample preparation of mycotoxins [151,152]. More efforts are needed to coordinate the optimization and the analytical performance of multidimensional separation techniques [65].…”

Determination of patulin in apple juice by amine‐functionalized solid‐phase extraction coupled with isotope dilution liquid chromatography tandem mass spectrometry

“…Among numbers of sample preparation methods, liquid–liquid extraction (LLE) by ethyl acetate, 11 QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction, 12,13 and solid‐phase extraction (SPE) 14 were the main strategies employed. It is noteworthy that SPE is becoming increasingly popular with better selectivity and repeatability in cleaning up and enrichment 15–18 . Many different adsorbents have therefore been utilized to develop sample pretreatment methods to minimize the matrix interferences from apple juice, including silica gel, 19 C 18 modified silica gel, 20 aminopropyl modified silica gel, 12 molecularly imprinted polymers (MIPs), 21,22 hydrophilic lipophilic balanced (HLB) cartridge, 23,24 and immunoaffinity columns (IACs) 25 .…”