Rapid determination of volatile benzene derivatives and chlorobenzenes in goat’s milk by HS-SPME-GC-MS/MS

A method for the determination of eight benzenes (BTEXs) and twelve chlorobenzenes (CBs) in goat's milk by headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS/MS) was developed. The study investigated the impact of various factors such as extraction fiber type, salt amount, equilibrium conditions, and desorption conditions on the outcomes. Target analytes were separated on a DB-HeavyWAX column and quantified using the external standard method. The results showed that the target compounds had a good linear relationship in the range of 0.01 ∼ 50 μg/L (<i>R</i>² > 0.997), the limit of detection (LOD) was 0.003 ∼ 0.150 μg/L, and the limit of quantification (LOQ) was 0.01 ∼ 0.50 μg/L. The average recoveries were 82%-116% and the relative standard deviation (RSD) was 0.8%-17.3% under the three addition levels of 1×, 2×, and 10 × LOQ. In a survey of twenty goat's milk samples, only ethylbenzene, xylenes, cumene, chlorobenzene, and 1,4-dichlorobenzene were detected at levels exceeding their respective limits of quantification. The method was evaluated using two ecological scales (Eco-Scale), GAPI and AGREEN, to verify its environmental friendliness and applicability. This method is simple, green, and efficient, which provides a certain theoretical basis for the production and quality safety evaluation of dairy products.