高效液相色谱-串联质谱法测定瓜果中11种植物生长调节剂的残留量

Determination of 11 Kinds of Plant Growth Regulator Residues in Fruits and Melons by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱（HPLC-MS/MS）法同时检测瓜果中多效唑、氯吡脲、异戊烯腺嘌呤、6-苄氨基嘌呤、2,4-二氯苯氧乙酸、赤霉素、吲哚-3-丁酸、α-萘乙酸、对氟苯氧乙酸、对氯苯氧乙酸和吲哚-3-乙酸11种植物生长调节剂的残留量.样品经乙腈提取、浓缩后,以Agilent XDB-C1s为分析色谱柱,5 mmol/L乙酸铵（含1‰甲酸）和乙腈作为流动相进行梯度洗脱分离,基质匹配标准溶液外标法定量.结果表明,11种植物生长调节剂在各自浓度范围内线性良好（r＞0.99）,以梨、西瓜和苹果为代表性基质进行3个水平加标回收实验,回收率为76.6％～ 119.0％,相对标准偏差低于9.1％,检出限在0.24～ 14.29 μg/kg之间.方法操作简便、耗时短、有机试剂使用量少、灵敏度高、稳定性好,应用于日常检测可大大降低检测成本,缩短检测周期,具有实际应用价值.

A method for the simultaneous determination of 11 plant growth regulator （PGR） residues in fruits and melons has been developed by using high performance liquid chromatography-tandem mass spectrometry （ HPLC-MS/MS ）. Paelobutrazol, forchlorfenuron, isopentennyladenine, 6-benzylaminopurine, 2,4-diehlorophenoxyacetic acid, gibberellie acid, indole-3-butyric acid, α-naphthaleneacetic acid, 4-fluorophenoxyacetic acid, 4-chlorophenoxyacetie acid and indole-3-acetie acid were concerned. Samples were extracted by acetonitrile and concentrated. The chromatographic analysis was carried out on an Agilent XDB-Cls column with 5 mmol/L ammonium acetate solution （contain 1%o formic acid） and aeetonitrile as the mobile phases in gradient program, and quantified by matrix-matched external standard method. The calibration curves showed good linearity in each range with correlation coefficients greater than 0.99. The limits of detections （ LODs, S/N〉3 ） were 0.24-14.29 txg/kg for the 11 PGRs spiked in pear, watermelon and apple. The recoveries of the 11 PGRs spiked at three levels ranged from 76.6% to 119.0%, with the relative standard deviations （RSDs） less than 9.1%. The method is simple, time-saving and environmental friendly with high sensitivity and good reproducibility, as well as having practical application value for its low- cost and short-circle.