Simultaneous determination of 28 illegal drugs in sewage by high throughput online SPE-ISTD-UHPLC-MS/MS

This study developed an online solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry (Online-SPE-UHPLC-MS/MS) method for the analysis of 28 illegal drugs in sewage. To achieve this, 28 isotope internal standards (ISTDs) were added to 3 mL sewage samples, the pH was adjusted to 7–8 using hydrochloric acid or 20% ammonia water, followed by centrifugation, filtration, and analysis using UHPLC-MS/MS. The results indicated an excellent linearity of 1–300 ng L −1 , and cotinine in the concentration range of 20–6000 ng L −1 , linear correlation coefficient R 2  > 0.995, with the limit of detection (LOD) of 0.01–6 ng L −1 , and a limit of quantification (LOQ) of 0.1–20 ng L −1 . The addition of three concentrates of low (2 ng L −1 /40 ng L −1 ), medium (20 ng L −1 /400 ng L −1 ), and high concentration (200 ng L −1 /4000 ng L −1 ) demonstrated the matrix effect of the target compound between ± 22.0%. The extraction recovery was 70.0–119.4%, and a percent accuracy of 75.7–118.1%. Similarly, the intra- and inter-day precisions were 1.8–20.0% and 1.5–18.9%, respectively. The results cemented the sensitivity, accuracy, reliability, strong specificity, and reproducibility, which can be used to screen 28 illegal drugs in sewage for trace analysis.