Development of a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using Soxtec device followed by gas chromatography-triple quadrupole tandem mass spectrometry

Abstract

Background: Organochlorinated compounds are major environmental concern due to their persistence, long-range transportability and bio-accumulation. Chlorinated paraffin (CP) mixtures, especially short-chain CPs (SCCPs), are found in environmental samples at very high levels. However, information about their levels is still insufficient, mainly in marine biota. Methods: This study aimed to optimize and validate a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using a Soxtec extractor and Gas Chromatography coupled with Mass Spectrometry in tandem GC-QqQ-MS/MS (EI). A Plackett-Burman (2^7*3/16) type III resolution factorial design was used to optimize the extraction and purification procedures, sample amount, extractant volume, boiling and rinsing times as extraction variables and alumina, acid silica gel amounts and elution volume as purification variables. Results: The most influent factors were sample amount, rinsing time, extractant volume and acid silica gel amount. Further experiments were performed in order to attain the optimal values of these factors (4 g sample amount, 50 mL n-hexane-dichloromethane as extractant volume, 2 and 1.5 h boiling and rinsing times, 8 g alumina, 4 g acid silica gel (15%) and 50 mL n-hexane-dichloromethane as elution solvent). Validation of the optimized method presented recoveries higher than 90% with RSD below 10%, showing good accuracy and precision. The whole method limits of detection and quantification were 46.13 mg Kg -1 and 153.75 mg Kg

Rapid Solid-Liquid Dynamic Extraction (RSLDE): A Powerful and Greener Alternative to the Latest Solid-Liquid Extraction Techniques

“…Nowadays, an improved method to perform Soxhlet extraction is named Soxtec [29]; this process is based on the same principles; however, thanks to pressure control, it is possible to accelerate the recirculation of the extractant solvent. In this way, the process is about 10 times faster [30].…”

A Quasi Real-Time Evaluation of High-Resolution Mass Spectra of Complex Chlorinated Paraffin Mixtures and Their Transformation Products

“…An aliquot of 10 mL was spiked with IS (20 ng) and dried with N 2 (30 °C). The sample was dissolved in n -hexane and added to a normal-phase chromatographic column containing activated silica (1.7 g), acidic silica (2.8 g, 40% sulfuric acid), and sodium sulfate . The column was washed with DCM (3 mL) and preconditioned with n -hexane (3 mL).…”

“…The sample was dissolved in n -hexane and added to a normal-phase chromatographic column containing activated silica (1.7 g), acidic silica (2.8 g, 40% sulfuric acid), and sodium sulfate. 26 The column was washed with DCM (3 mL) and preconditioned with n -hexane (3 mL). Two fractions were obtained after the column was rinsed with n -hexane (Fr.…”

Determination and analysis of harmful components in synthetic running tracks from Chinese primary and middle schools

“…The oven temperature program was 90 °C (1 min), 25 °C·min −1 to 150 °C and 8 °C·min −1 to 300 °C (15 min). Other measurement parameters of the instrument were provided in a recent publication 37 .…”