An effective method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and optimized to obtain a complete separation of five representative plant growth regulators (PGRs) [gibberellic acid, 2,4-dichlorophenoxyacetic acid (2,4-D), thidiazuron, forchlorfenuron, and paclobutrazol] in fruits. Extraction was performed with acetonitrile containing 0.1% (v/v) acetic acid, applying modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) methodology. LC-MS/MS conditions including composition of mobile phases and mass spectrometry (MS) conditions were evaluated to achieve the highest sensitivity in MS detection. All of the data acquisition was employed in the segmented multiple-reaction monitoring mode for the selected negative and positive transition ions. The octadecylsilyl (C18) dispersive solid-phase extraction (SPE) sorbent was found to provide the more satisfied recoveries than primary secondary amine (PSA) and graphitized carbon black (GCB) for five target PGRs. The optimized method allowed for recoveries of 76-112% for the five PGRs from fruit samples with relative standard deviation (RSD) values less than 10%. Limits of quantification (0.5-16.5 μg/kg) were lower than the maximum limit of residues established for PGRs. The results demonstrated that the developed LC-MS/MS and QuEChERS extraction method is highly effective for analyzing trace amounts of target PGRs in fruit samples. Finally, the method was successfully used to detect residual PGRs in Beijing, China, in 2010. The concentrations of 2,4-D (5.1-1503 μg/kg) and paclobutrazol (1-1381 μg/kg) found in orange and peach, respectively, suggesting that the use of these PGRs in these fruits should be regulated in China in the future.

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An improved method for solid-phase extraction (SPE)–liquid chromatography–tandem mass spectrometry was developed to analyze eight monoalkyl phthalate esters (MPEs) in eight different kinds of porcine tissues. The tissue samples were processed using enzymatic deconjugation with β-glucuronidase, followed by SPE with Oasis MAX cartridges. A pentafluorophenyl column was first used to solve the coeluting issues of MPE isomers. The limits of detection and recoveries were 0.01–0.6 ng/g and 62.5–123.7%, respectively. The intra- and interday precisions were less than 7.1 and 9.4%, respectively. The robust method was successfully applied for the investigation of MPEs in various porcine tissue samples collected from markets in Beijing, China. The occurrence of MPEs with total concentrations of 48.0–108 ng/g was detected, and monoethylhexyl phthalate was the predominant MPE (accounting for 30–57%) in all of the porcine tissue samples. The results will be helpful in assessing the potential risks of diets that include pork.