RESUMEN
A simple, accurate, and highly sensitive analytical method was developed in this study for the determination of ten ß-agonists and five ß-blockers in milk. In this method, new adsorbent phosphonic acid-functionalized porous organic polymers were synthesized through a direct knitting method. The synthesis procedure of the materials and the extraction conditions (such as the composition of loading buffer and eluent) were optimized. Benefitting from the high surface area (545-804 m2 g-1), multiple functional framework and good porosity, the phosphonic acid-functionalized porous organic polymers showed a high adsorption rate and high adsorption capacity for ß-agonists (224 mg g-1 and 171 mg g-1 for clenbuterol and ractopamine, respectively). The analytes were quantified by ultra-high-performance liquid chromatography coupled to high-resolution tandem mass spectrometry. It showed a good linearity (with R 2 ranging from 0.9950 to 0.9991 in the linear range of 3-5 orders of magnitude), with low limits of quantification ranging from 0.05 to 0.25 ng g-1. The limits of detection of the method for the analytes were measured to be in the range of 0.02 to 0.1 ng g-1. The recoveries of target analytes from real samples on the material were in the range of 62.4-119.4% with relative standard deviations of 0.6-12.1% (n = 4). Moreover, good reproducibility of the method was obtained with the interday RSD being lower than 11.7% (n = 5) and intraday RSD lower than 12.2% (n = 4). The proposed method was accurate, reliable and convenient for the simultaneous analysis of multiple ß-agonists and ß-blockers. Finally, the method was successfully applied for the analysis of such compounds in milk samples.
RESUMEN
An effective method based on ultra-high performance liquid chromatography-triple quadrupole/electrostatic field orbitrap mass spectrometry (UHPLC-Q-Orbitrap MS) was developed for high-throughput screening and quantitative analysis of 112 pharmaceutical and personal care products (PPCPs) in water. The water samples were separately extracted under alkaline and acidic conditions and cleaned on an SPE column (Cleanert PEP-2). The sample was separated and detected by UHPLC-Q-Orbitrap MS, and the data were collected in full MS scan/date dependent MS2 mode. All the 112 PPCPs in water were qualitatively screened and quantified on the basis of the peak area of the precursor ion. The PPCPs showed a good linear response in the mass concentration range of three orders of magnitude (r2 ≥ 0.9901), and the limits of quantification were between 0.002 µg/L and 0.8 µg/L. The recoveries of 60.1%-129.5% were achieved at different spiked levels of 0.2, 0.4, and 0.8 µg/L, and the RSDs were 1.1%-17.8% (n=6). Moreover, the method was used to screen the PPCPs in water samples acquired from seven regions of Dalian city (China), and 16 PPCPs were identified and quantified. Therefore, this simple method with high sensitivity and wide screening range can be applied to water quality management and environmental risk monitoring.