Simultaneous determination of selected estrogenic endocrine disrupting chemicals and bisphenol A residues in whole milk using fabric phase sorptive extraction coupled to HPLC‐UV detection and LC‐MS/MS

Abstract

A simple and sensitive analytical methodology is developed for rapid screening and quantification of selected estrogenic endocrine disrupting chemicals and bisphenol A from intact milk using fabric phase sorptive extraction in combination with high‐performance liquid chromatography coupled to ultraviolet detection/tandem mass spectrometry. The new approach eliminates protein precipitation and defatting step from the sample preparation workflow. In addition, the error prone and time‐consuming solvent evaporation and sample reconstitution step used as the sample post‐treatment has been eliminated. Parameters with most significant impact on the extraction efficiency of fabric phase sorptive extraction including sorbent chemistry, sample volume, extraction time have been thoroughly studied and optimized. Separation of the selected estrogenic endocrine disrupting chemicals including α‐estradiol, hexestrol, estrone, 17α‐ethinyl estradiol, diethylstilboestrol, and bisphenol A were achieved using a Zorbax Extend‐C18 high‐performance liquid chromatography column (15 cm × 4.6 mm, 5 μm particle size). The limit of detection values obtained in fabric phase sorptive extraction with high‐performance liquid chromatography with ultraviolet detection ranged from 25.0 to 50.0 ng/mL. The method repeatability values were 3.6–13.9 (relative standard deviation, %) and intermediate precision values were 4.6–12.7 (relative standard deviation, %). The fabric phase sorptive extraction method was also coupled to liquid chromatography with tandem mass spectrometry for identifying each endocrine disrupting chemical at 10 ng/mL.

Homoisoflavonoids profiling of Ophiopogon japonicus by off‐line coupling high‐speed countercurrent chromatography with high‐performance liquid chromatography–diode array detector‒quadrupole time‐of‐flight tandem mass spectrometry

“…It was reported that about 50 homoisoflavoniods were purified and identified by repeated column fractionations [1]. HPLC with diode array detector (DAD) and MS/MS has been developed for rapid isolation and characterization of bioactive components from complex natural products [8–11]. However, information about comprehensive analysis of homoisoflavonoids, especially for minors, in O. japonicus by HPLC–DAD–MS/MS is restricted because of the existence of multicomponents, restriction of detection sensitivity, and coelution of minor and abundant compounds [12,13].…”

Monodisperse restricted access material with molecularly imprinted surface for selective solid‐phase extraction of 17β‐estradiol from milk

“…The adsorption capacity of the adsorbents to four structural analogues (17α-E 2 , E 3 , E 1 , and DES; Supporting Information Figure S1) were determined in the same way. Additionally, the imprinting factor (IF) and selectivity coefficient (SC) are defined according to Equations (8) and (9) [29]:…”

“…Therefore, to ensure food safety and human health, it is necessary to find a simple and efficient analytical method for detecting the residual amount of 17β-E 2 in animal-derived foods. Due to the complexity of food matrices and the low concentration of 17β-E 2 in foods [7,8], effective pretreatment procedures, such as LLE [9], SPE [10], and SPME [11], are usually necessary to enable detection of 17β-E 2 . Of these, SPE is the most widely applied technique in recent years.…”

A Novel Electrochemical Sensor Based on FeNi3/CuS/ BiOCl Modified Carbon Paste Electrode for Determination of Bisphenol A

“…Therefore, designing a sensitive and simple technique to detect BPA would be of special importance. Some analytical procedures have been utilized in determination of BPA such as the gas chromatography‐mass spectrometry (GC‐MS) [5], enzyme‐linked immuno‐sorbent assay (ELISA) [6], HPLC [7], optical sensor [8], fluorescent [9], electrochemical [10], and colorimetric sensors [11]. Although they can provide highly sensitive detection and accurate identification, a majority of the mentioned techniques suffer from a number of limitations like the necessity of the pretreatment stages, very high time consumption, and expensiveness.…”