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苹果中萘乙酸残留量的高压液相色谱测定法

High pressure liquid chromatographic determination of naphthaleneacetic acid residues in apples.

作者信息

Cochrane W P, Lanouette M

出版信息

J Assoc Off Anal Chem. 1979 Jan;62(1):100-6.

PMID:422492
Abstract

An ion-suppression reverse phase high pressure liquid chromatographic method is described for determining naphthaleneacetic acid (NAA) residues in apples. Samples are extracted with acidic chloroform, filtered through pre-acidified Hy-Flo Supercel, and cleaned up by acid-base partitioning. The extract can be successfully chromatographed on either a muLiChrosorb NH2 or muBondapak C18 column and quantitated by using a variable wavelength ultraviolet detector set at 220 nm. The mobile phase is acetonitrile-water (20 + 80) buffered to pH 3.5 (MULiChrosorb column) or pH 5.2 (MUBondapak column) and flowing at 1.0--2.0 ml/min. Recoveries ranged from 86 to 98%. The minimum detectable amount was 0.5 ng, which easily permitted the quantitation of 0.01 ppm NAA in 50 g sample. A fluorometric detector was 4 times as sensitive, using an excitation wavelength of 220 mm and monitoring the emission at 340 nm. For this detector, the minimum detectable amount was 0.12 ng NAA.

摘要

本文描述了一种离子抑制反相高压液相色谱法,用于测定苹果中萘乙酸(NAA)残留量。样品用酸性氯仿萃取,通过预酸化的硅藻土助滤剂过滤,并通过酸碱分配进行净化。提取物可在μLiChrosorb NH2或μBondapak C18柱上成功进行色谱分析,并使用设置在220 nm的可变波长紫外检测器进行定量。流动相为乙腈 - 水(20 + 80),缓冲至pH 3.5(μLiChrosorb柱)或pH 5.2(μBondapak柱),流速为1.0 - 2.0 ml/min。回收率在86%至98%之间。最低检测量为0.5 ng,这使得在50 g样品中能够轻松定量0.01 ppm的NAA。荧光检测器的灵敏度是紫外检测器的4倍,激发波长为220 nm,监测发射波长为340 nm。对于该检测器,最低检测量为0.12 ng NAA。

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