【求助】求助四聚乙醛分析方法

你好！四聚乙醛的文献只找到两篇相关分析的，您参考一下吧：

[url=https://insevent.instrument.com.cn/t/Mp]气相色谱法测定密达颗粒剂中的四聚乙醛[/url]
四聚乙醛在烟草和土壤中的残留检测与消解动态

应助达人

四聚乙醛日本官方方法是用GCMS检测的.网上查到的也是这样,定量粒子是89.你可以让有关系的查一下日本官方方法.这样做起来比较方便.

应助达人

在前处理时:我们试过用三氯甲烷萃取,Carb/NH2除杂质,回收还行,可就是基底不能是毛豆,三氯甲烷萃取出来的油实在是太多了,只称2克都有不少油的.

应助达人

如果可能的话,能发上来参考参考吗?

四聚乙醛（metaldehyde）的检测方法
1.Determination of metaldehyde residues in various vegetables through HPLC.
Aitzetmueller, K | Fox, J | Arzberger, E | Schoettler, H
Deutsche Lebensmittel-Rundschau [DTSCH. LEBENSM.-RUNDSCH.]. Vol. 80, no. 7, pp. 201-203. 1984.

A method for the quantitative determination of metaldehyde residues in vegetables by HPLC was developed. Metaldehyde is extracted with toluene from plant substrates and then depolymerized by acid and, in a two-phase reaction, derivatized to the dinitrophenyl hydranzone of acetaldehyde. This is separated from interfering substances and quantitatively determined by way of gradient-elution HPLC on silica with UV detection.

http://md1.csa.com/partners/viewrecord.php?requester=gs&collection=ENV&recid=1023547&q=determination+of+metaldehyde+&uid=&setcookie=yes

2.Determination of metaldehyde in human serum by headspace solid-phase microextraction and gas chromatography–mass spectrometry
Takeshi Saito, et al.;
Journal of Chromatography B;Volume 875, Issue 2, 15 November 2008, Pages 573-576

Abstract:
A rapid headspace solid-phase microextraction–gas chromatography–mass spectrometry (HS–SPME–GC–MS) method has been developed for the determination of metaldehyde in human serum samples. Metaldehyde is extensively used as a molluscicide for the control of slugs and snails, and cases of metaldehyde poisoning have been reported. Metaldehyde was headspace-extracted on a polydimethylsiloxane (PDMS) fiber at 70 °C for 25 min, desorbed, and analyzed rapidly by GC–MS. The method was validated for limit of detection (LOD), linearity, precision, and recovery. Although the recovery of the sample was very low, the method itself was rapid with a low detection limit of 0.25 μg/ml, R.S.D. value 12.6%, and linearity range 0.5–25.0 μg/ml (r² = 0.999). The results demonstrated that the SPME–GC–MS method for the analysis of metaldehyde is simple, rapid, solvent-free, and does not require any pre-analysis conversions.

http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6X0P-4TMSNVN-2&_user=10&_rdoc=1&_fmt=&_orig=search&_sort=d&view=c&_acct=C000050221&_version=1&_urlVersion=0&_userid=10&md5=c70bffac7bf24cda50c31cd501d000c2