College of Science, China Agricultural University, Beijing 100193, PR China.
Rapid Commun Mass Spectrom. 2011 Nov 15;25(21):3289-97. doi: 10.1002/rcm.5225.
A sensitive and rapid multi-residue analytical method for plant growth regulators (PGRs) (i.e., chlormequat, mepiquat, paclobutrazol, uniconazole, ethephon and flumetralin) in apples and tomatoes was developed using high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). A homogenised sample was extracted with a mixture of methanol/water (90:10, v/v) and adjusted to pH <3 with formic acid. Primary secondary amine (PSA) adsorbent was used to clean up the sample. The determination was performed using electrospray ionisation (ESI) and a triple quadrupole (QqQ) analyser. Under the optimised method, the results showed that, except for ethephon, the recoveries were 81.8-98.1% in apples and tomatoes at the spiked concentrations of 0.005 to 2 mg/kg, with relative standard deviations (RSDs) of less than 11.7%. The limits of quantification (LOQs) were lower than their maximum residue limits (MRLs). The procedure was concluded as a practical method to determine the PGR residues in fruit and vegetables and is also suitable for the simultaneous analysis of the amounts of samples for routine monitoring. The analytical method described herein demonstrates a strong potential for its application in the field of PGR multi-residue analysis to help assure food safety.
建立了一种采用高效液相色谱/串联质谱(HPLC/MS/MS)检测苹果和番茄中植物生长调节剂(PGRs)(即矮壮素、甲哌𬭩、多效唑、烯效唑、乙烯利和氟节胺)残留的灵敏、快速的多残留分析方法。将均质化的样品用甲醇/水(90:10,v/v)混合液提取并用甲酸调节 pH 值<3。采用初级二级胺(PSA)吸附剂对样品进行净化。测定采用电喷雾离子化(ESI)和三重四极杆(QqQ)分析器。在优化的方法条件下,结果表明,除乙烯利外,在苹果和番茄中,0.005-2mg/kg 浓度添加水平下,除乙草胺外,其余 7 种 PGR 的回收率为 81.8-98.1%,相对标准偏差(RSD)小于 11.7%。定量限(LOQs)均低于其最大残留限量(MRLs)。该程序被认为是一种实用的方法,可用于测定水果和蔬菜中的 PGR 残留,也适合于常规监测的大量样品的同时分析。本文所描述的分析方法在 PGR 多残留分析领域具有很强的应用潜力,有助于确保食品安全。