Microwave Assisted Cloud Point Extraction for the Determination of Vitamin K Homologues in Vegetables by Liquid Chromatography with Tandem Mass Spectrometry

Abstract

Liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) with a triple quadrupole (QqQ) is proposed for determining the vitamin K homologues, phylloquinone (PK), menaquinone-4 (MK) and menadione (MD), in vegetables. The analytes were isolated from the samples (1−1.5 g) by ultrasound assisted extraction using acetonitrile (2 mL), and the liquids were submitted to microwave assisted cloud point extraction with Triton X-45. The enrichment factors were between 20 and 50, depending on the vitamin homologue in question. The analytes were determined by LC-ESI-QqQ-MS/MS in the multiple reaction monitoring (MRM) mode, providing unequivocal identification and quantification, with limits of detection of 0.8, 1.0, and 16 ng/g for MK, PK, and MD, respectively. Recovery assays for samples spiked at two concentration levels, between 40 and 600 ng/g depending on the compound, provided recoveries in the 90−114% range. Only PK was detected in the samples analyzed, at concentrations in the 90−2350 ng/g range.

Updating the Status quo on the Eco-Friendly Approach for Antioxidants Recovered from Plant Matrices Using Cloud Point Extraction

“…This is additional proof that this technique surely requires more investigation and optimization, compared with the ultrasound-coupled extraction procedure, since researchers did not make a greater contribution in this field. As shown in Table 5 , Campillo et al [ 67 ] explored the CPE-MAE for recovery of vitamin K from vegetables (iceberg lettuce, romaine lettuce, lamb’s lettuce, escarole lettuce, kale, spinach, cress, turnip, parsnip, and carrot). A similar study was conducted by Yu et al [ 68 ] in order to determine polyphenols and furocoumarins from fig leaves.…”

Recent advances of green pretreatment techniques for quality control of natural products

“…A few non-ionic surfactants were employed for extracting NPs by CPE extraction procedure, such as Genapol X-080, Tween 80, SPAN 80, Triton X-45, Triton X-114, Tergitol TMN-6, etc. Assistant mode also be introduced for enhancing the extraction efficiency, such as microwave assisted CPE [97] and ultrasound assisted integrative CPE [98]. In addition, synergistic CPE was also proposed by Zhou et al to simplify the extraction and detection of isoquercitrin, which owns a few pharmacological and biological activities and has been considered to have therapeutic actions [99].…”

Simultaneous Determination of Six Isoflavones from Puerariae Lobatae Radix by CPE-HPLC and Effect of Puerarin on Tyrosinase Activity

“…Cloud-point extraction has been reported in many studies concerning the extraction and preconcentration of solutes from water [22], urine [23], and soil [24]. However, little was known about the use of surfactant solution as a solvent for the extraction of chemical constituents from herbal products [25,26].…”