Mou Yanli, Guo Dehua, Ding Zhuoping
College of Food Science & Technology, Shanghai Ocean University, Shanghai 201306, China.
Shanghai Exit-Entry Inspection and Quarantine Bureau, Shanghai 200135, China.
Se Pu. 2013 Oct;31(10):1016-20. doi: 10.3724/sp.j.1123.2013.06003.
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of the plant growth regulator (PGR) (paclobutrazol, forchlorfenuron, isopentennyladenine and 6-benzylaminopurine) residues in amphisarcas. The sample was extracted with acetonitrile, then cleaned up by MCX solid phase extraction. The HPLC separation was performed on an Agilent XDB-C18 column with 5 mmol/L ammonium acetate solution and acetonitrile containing 0.1% (volume percentage) formic acid as the mobile phases in a gradient elution mode. The PGRs were determined by MS/MS in positive electrospray ionization mode, and quantified by matrix-matched external standard method. The calibration curves showed good linearity in each range with correlation coefficients greater than 0.999. The limits of quantification (LOQs, S/N > 10) were 0.04-1.35 g/kg and the limits of detection (LODs, S/N > 3) were 0. 01-0 41 microg/kg for the four PGRs spiked in cucumber and apple. The recoveries of the four PGRs spiked at three levels ranged from 81.0% to 93.%, with the relative standard deviations (RSDs) of 3.5%-9.5%. The sensitivity, accuracy and precision of the method meet the technical standards of the pesticide determination. Therefore the method can be applied to the determination of the four PGRs in amphisarcas.
建立了一种高效液相色谱 - 串联质谱法(HPLC - MS/MS)用于测定两栖蓼中植物生长调节剂(PGR)(多效唑、氯吡脲、异戊烯腺嘌呤和6 - 苄氨基嘌呤)的残留量。样品用乙腈提取,然后通过MCX固相萃取进行净化。HPLC分离在Agilent XDB - C18柱上进行,以5 mmol/L醋酸铵溶液和含0.1%(体积百分比)甲酸的乙腈为流动相,采用梯度洗脱模式。PGR通过正电喷雾电离模式下的MS/MS测定,并采用基质匹配外标法进行定量。校准曲线在各个范围内均显示出良好的线性,相关系数大于0.999。添加到黄瓜和苹果中的四种PGR的定量限(LOQs,S/N > 10)为0.04 - 1.35 μg/kg,检测限(LODs,S/N > 3)为0.01 - 0.41 μg/kg。三种添加水平下四种PGR的回收率在81.0%至93.0%之间,相对标准偏差(RSDs)为3.5% - 9.5%。该方法的灵敏度、准确度和精密度符合农药测定的技术标准。因此,该方法可用于测定两栖蓼中四种PGR的残留量。