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[基于QuEChERS-高效液相色谱-串联质谱法测定水果中21种植物生长调节剂残留量]

[Determination of 21 plant growth regulator residues in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry].

作者信息

Huang Hehe, Zhang Jin, Xu Dunming, Zhou Yu, Luo Jia, Li Meiling, Chen Shubin, Wang Lianzhu

出版信息

Se Pu. 2014 Jul;32(7):707-16. doi: 10.3724/sp.j.1123.2014.03003.

Abstract

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, forchlorfenuron, thidiazuron, inabenfide, paclobutrazol, uniconazole and triapenthenol were in the concentration range of 0.1-500 microg/L, daminozide and 6-benzylaminopurine in the concentration range of 1.0-500 microg/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 microg/L, abscisic acid (ABA), gibberellic acid (GA3), 1-naphthaleneacetic acid (NAA) and indol-3-ylacetic acid (IAA) in the concentration range of 10-1000 microg/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 microg/kg and 0.10-15.0 microg/kg, respectively. For all the samples, the average spiked recoveries 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.

摘要

建立了一种采用QuEChERS-高效液相色谱-串联质谱法(HPLC-MS/MS)同时检测水果中21种植物生长调节剂的方法。样品先用含1%(v/v)乙酸的乙腈提取,然后用硫酸镁和C18粉末净化。所得样品在C18柱上分离,并通过时间段之间的极性切换在正、负离子多反应监测(MRM)模式下进行检测。采用基质匹配外标校准曲线进行定量分析。氯化氯胆碱、甲哌鎓、氯化胆碱、环丙酰草胺、氯吡脲、噻苯隆、异稻瘟净、多效唑、烯效唑和调环醇的线性范围为0.1 - 500 μg/L,氨基丁三醇和6-苄氨基嘌呤的线性范围为1.0 - 500 μg/L,2,3,5-三碘苯甲酸、2,4-滴、矮壮素、4-氯苯氧乙酸(4-CPA)和抗倒酯的线性范围为2.0 - 1000 μg/L,脱落酸(ABA)、赤霉酸(GA3)、1-萘乙酸(NAA)和吲哚-3-乙酸(IAA)的线性范围为10 - 1000 μg/L,相关系数均高于0.990。该方法的检出限和定量限分别为0.020 - 6.0 μg/kg和0.10 - 15.0 μg/kg。对于所有样品,平均加标回收率在73.0%至111.0%之间,相对标准偏差(RSD,n = 6)在3.0% - 17.2%范围内。该方法快速、简便、有效、灵敏且准确,能够满足水果中21种植物生长调节剂残留量测定的要求。

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