Simultaneous Determination of Five Plant Growth Regulators in Fruits by Modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Extraction and Liquid Chromatography–Tandem Mass Spectrometry

• Published in: Journal of agricultural and food chemistry Vol. 60; no. 1; pp. 60 - 65
• Main Authors: Shi, Xiaomei, Jin, Fen, Huang, Yuting, Du, Xinwei, Li, Chunmei, Wang, Miao, Shao, Hua, Jin, Maojun, Wang, Jing
• Format: Journal Article
• Language: English
• Published: Washington, DC American Chemical Society 11.01.2012
• Subjects: 2,4-D; acetic acid; Biological and medical sciences; carbon; Chromatography, High Pressure Liquid - economics; Chromatography, High Pressure Liquid - methods; Food Contamination - analysis; Food engineering; Food industries; forchlorfenuron; Fruit - chemistry; Fruit and vegetable industries; fruits; Fundamental and applied biological sciences. Psychology; General aspects; gibberellic acid; ions; mass spectrometry; maximum residue limits; monitoring; paclobutrazol; peaches; Plant Growth Regulators - analysis; solid phase extraction; Solid Phase Extraction - economics; Solid Phase Extraction - methods; Tandem Mass Spectrometry - economics; Tandem Mass Spectrometry - methods; thidiazuron; China; Plant growth regulators; fruits; liquid chromatography−tandem mass spectrometry; QuEChERS extraction; Fruit; liquid chromatography-tandem mass spectrometry; Plant growth substance; Liquid chromatography; Extraction; Mass spectrometry
• ISSN: 0021-8561; 1520-5118
• DOI: 10.1021/jf204183d

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.