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建立了高效液相色谱-串联质谱法( HPLC-MS/MS)同时测定水果中21种植物生长调节剂残留量的方法。样品经 QuEChERS法进行预处理,选用含1%( v/v)乙酸的乙腈溶液提取,无水硫酸镁和十八烷基硅烷( C18)粉末净化,以 C18色谱柱分离待测物,采用鞘流电喷雾离子化,正负离子分段扫描和多反应监测模式( MRM)检测,基质匹配标准溶液外标法定量。矮壮素、助壮素、氯化胆碱、环丙酸酰胺、氯吡脲、噻苯隆、抗倒胺、多效唑、烯效唑和抑芽唑在0.10~500μg/L,丁酰肼和6-苄氨基嘌呤在1.0~500μg/L,2,3,5-三碘苯甲酸、2,4-D、调果酸、对氯苯氧乙酸(4-CPA)和抗倒酯在2.0~1000μg/L,赤霉素(GA3)、脱落酸(ABA)、1-萘乙酸(NAA)和吲哚-3-乙酸(IAA)在10~1000μg/L的范围内线性关系良好,相关系数均大于0.990。21种植物生长调节剂的方法检出限为0.020~6.0μg/kg,方法定量限为0.10~15.0μg/kg,样品添加回收试验的平均回收率为73.0%~111.0%,相对标准偏差为3.0%~17.2%( n=6)。该方法快速简便,定量准确,可满足多种水果中21种植物生长调节剂的残留检测要求。

A method for the simultaneous detection of 21 plant growth regulators in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS)was developed. The samples were initially extracted with acetonitrile containing 1%( v/v) acetic acid,followed by clean-up using the powder of magnesium sulfate and C18. The resulting samples were separated on a C18 column,and detected under positive and negative multiple reactions monitoring( MRM ) mode through polarity switching between time segments. The matrix-matched external standard calibration curves were used for quantitative analysis. The linearities of chlormequat chloride,mepiquat chloride,choline chloride,cyclanilide,forchlor-fenuron,thidiazuron,inabenfide,paclobutrazol,uniconazole and triapenthenol were in the concentration range of 0. 1-500 μg/L,daminozide and 6-benzylaminopurine in the concentra-tion range of 1. 0-500 μg/L,2,3,5-triiodobenzoic acid,2,4-D,cloprop,4-chlorophenoxyacetic acid(4-CPA)and trinexapac-ethyl in the concentration range of 2. 0-1 000 μg/L,abscisic acid (ABA),gibberellic acid(GA3),1-naphthaleneacetic acid(NAA)and indol-3-ylacetic acid (IAA)in the concentration range of 10-1 000 μg/L,with the correlation coefficients higher than 0. 990. The limits of detection and the limits of quantification of the method were 0. 020-6. 0 μg/kg and 0. 10-15. 0 μg/kg,respectively. For all the samples,the average spiked recover-ies ranged from 73. 0% to 111. 0%,and the relative standard deviations( RSDs,n=6)were in the range of 3. 0%-17. 2%. The method is quick,easy,effective,sensitive and accurate,and can meet the requirements for the determination of the 21 plant growth regulator residues in fruits.

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