Solid-phase microextraction for organochlorine pesticide residues analysis in Chinese herbal formulations

Solid-phase microextraction (SPME) coupled with gas chromatography–mass spectrometry (GC–MS) was used to determine pesticide residues in Chinese herbal formulations. Fibers coated with a 100-μm film thickness of poly(dimethylsiloxane) was used to extract 19 organochlorine pesticides (OCPs). The pesticides in the study consisted of α-, β-, γ- and δ-hexachlorocyclohexane, p,p′-DDD, p,p′-DDE, p,p′-DDT, o,p′-DDT, aldrin, dieldrin, endrin, endrin aldehyde, endrin ketone, endosulfan (I, II and sulfate), heptachlor, heptachlor epoxide, and methoxychlor. The optimal experimental procedures for the adsorption and desorption of pesticides were evaluated. The linearity was obtained with a precision below 11% RSD for the studied pesticides expect endosulfan sulfate (21%) in a wide range from 1 to 200 ng/g. Detection limits were reached at below ng/g levels. Heptachlor epoxide was determined at a calculated limit of 0.03 ng/g. Comparison between SPME and Soxhlet extraction showed that SPME has a less than one order detection limit for residue pesticide determination. The proposed method was tested by analyzing herbal formulations from a local market for OCP multi-residues. Some residues studied were detected in the analyzed samples. The results demonstrate the suitability of the SPME–GC–MS approach for the analysis of multi-residue OCPs in Chinese herbal formulations.