【分享】柱后衍生分析氨基甲酸酯、霉菌毒素等的方法

楼主您好 我们最近刚开始柱后衍生荧光法测定 氨基甲酸酯手头的资料有限 一直做的不理想，不知能否参考一下楼主的？

以下是真菌毒素（mycotoxins）的检测方法，有些有全文，有些有链接。

Determination of mycotoxins
Hans P. vanEgmond & Walter H. Paulsch
Pure &AppI. Chem., Vol. 58, No. 2, pp. 315—326, 1986.
Printed in Great Britain.

Abstract:
Various approaches exist to the determination of mycotoxins. Chemical assays are of major importance. Generally, all chemical analytical methods for the determination of mycotoxins include the basic steps of extraction, clean—up, separation, detection, quantitation and confirmation of identity. Most widely used are those techniques which include a chromatographic step to separate the mycotoxin of interest (minicolumn chromatography, thin layer chromatography, high performance liquid chromatography and gas liquid chromatography). Immuno—assays, which are bio—chemical separation techniques, are promising but still in an early stage of development for mycotoxin research.

Determination of mycotoxins

Recent advances in mycotoxin determination in food and feed by hyphenated chromatographic techniques/mass spectrometry
SFORZA Stefano,et al.,
Mass spectrometry reviews, 2006, vol. 25, no1, pp. 54-76 [23 page(s) (article)] (2 p.1/4)
Abstract:
Mycotoxins are fungal toxins produced by molds, which occur universally in food and feed derivatives, and are produced under certain environmental conditions in the field before harvest, post-harvest, during storage, processing, and feeding. Mycotoxin contamination is one of the most relevant and worrisome problem concerning food and feed safety because it can cause a variety of toxic acute and chronic effects in human and animals. In this review we report the use of mass spectrometry in connection with chromatographic techniques for mycotoxin determination by considering separately the most diffuse class of mycotoxins: patulin, aflatoxins, ochratoxinA, zearalenone, trichothecenes, and fumonisins. Although the selectivity of mass spectrometry is unchallenged if compared to common gc and $$lc detection methods, accuracy, precision, and sensitivity may be extremely variable concerning the different mycotoxins, matrices, and instruments. The sensitivity issue may be a real problem in the case of$$lc/MS, where the response can be very different for the different ionization techniques (ESI, APCI, APPI). Therefore, when other detection methods (such as fluorescence or UVabsorbance) can be used for the quantitative determination, $$lc/MS appears to be only an outstanding confirmatory technique. In contrast, when the toxins are not volatile and do not bear suitable chromophores or fluorophores, $$lc/MS appears to be the unique method to perform quantitative and qualitative analyses without requiring any derivatization procedure. The problem of exact quantitative determination in gc/MS and $$lc/MS methods is particularly important for mycotoxin determination in food, given the high variability of the matrices, and can be solved only by the use of isotopically labeled internal standards or by the use of ionization interfaces able to lower matrix effects and ion suppressions. When the problems linked to inconstant ionization and matrix effects will be solved, only MS detectors will allow to simplify more and more the sample preparation procedures and to avoid clean-up procedures, making feasible low-cost, high-throughput determination of mycotoxins in many different food matrices.

http://cat.inist.fr/?aModele=afficheN&cpsidt=17445512
http://www.biomedexperts.com/Abstract.bme/15892148/Recent_advances_in_mycotoxin_determination_in_food_and_feed_by_hyphenated_chromatographic_techniques_mass_spectrometry

Analytical methods for determination of mycotoxins: a review.
Turner NW, Subrahmanyam S, Piletsky SA.
Anal Chim Acta. 2009 Jan 26;632(2):168-80. Epub 2008 Nov 14

Abstract:
Mycotoxins are small (MW approximately 700), toxic chemical products formed as secondary metabolites by a few fungal species that readily colonise crops and contaminate them with toxins in the field or after harvest. Ochratoxins and Aflatoxins are mycotoxins of major significance and hence there has been significant research on broad range of analytical and detection techniques that could be useful and practical. Due to the variety of structures of these toxins, it is impossible to use one standard technique for analysis and/or detection. Practical requirements for high-sensitivity analysis and the need for a specialist laboratory setting create challenges for routine analysis. Several existing analytical techniques, which offer flexible and broad-based methods of analysis and in some cases detection, have been discussed in this manuscript. There are a number of methods used, of which many are lab-based, but to our knowledge there seems to be no single technique that stands out above the rest, although analytical liquid chromatography, commonly linked with mass spectroscopy is likely to be popular. This review manuscript discusses (a) sample pre-treatment methods such as liquid-liquid extraction (LLE), supercritical fluid extraction (SFE), solid phase extraction (SPE), (b) separation methods such as (TLC), high performance liquid chromatography (HPLC), gas chromatography (GC), and capillary electrophoresis (CE) and (c) others such as ELISA. Further currents trends, advantages and disadvantages and future prospects of these methods have been discussed.

http://www.ncbi.nlm.nih.gov/pubmed/19110091

1.
Determination of selected mycotoxins in mould cheeses with liquid chromatography coupled to tandem with mass spectrometry
Kokkonen, Meri, et al.,
Food Additives and Contaminants, Volume 22, Number 5, May 2005 , pp. 449-456(8)

Abstract:
A simple and feasible method is described for analysing nine mycotoxins in cheese matrix. The method involves liquid extraction followed by high performance liquid chromatographic separation and mass spectrometric detection of the analytes, and allows the determination of aflatoxins B1, B2, G1, G2 and M1, ochratoxin A, mycophenolic acid, penicillic acid and roquefortine C simultaneously. Average recoveries of the mycotoxins from spiked samples at concentration levels of 5–200?µg?kg -1 ranged from 96–143%. Within-day relative standard deviations at these concentration levels varied from 2.3–12.1%. The limit of quantification for aflatoxin M1 was 0.6?µg?kg -1 and for the other compounds 5?µg?kg -1 . The method developed was applied for analysing these mycotoxins in blue and white mould cheeses purchased from Finnish supermarkets. Roquefortine C was detected in all of the blue mould cheese samples in concentrations of 0.8–12?mg?kg -1 . One blue cheese contained also 0.3?mg?kg -1 mycophenolic acid. The other investigated mycotoxins were absent in the samples.
http://www.ingentaconnect.com/content/tandf/tfac/2005/00000022/00000005/art00008;jsessionid=2dclmsndn0pi0.alexandra

2.
Determination of Mycotoxin and Mycotoxin Metabolites using LC/MS/MS

黄曲霉毒素（Aflatoxin）的检测方法有：

1.
GB/T 5009.23—1996 食品中黄曲霉毒素B1、B2、G1、G2的测定方法
全文链接： http://www.foodqs.com/news/jcbz04/2003821141656.htm

2.
COMPARISON OF METHODS BY TLC AND HPTLC FOR DETERMINATION OF AFLATOXIN M1 IN MILK AND B1 IN EGGS
V.M.Scussel


全文

3.
戴安的资料：
Fast and Effective Determination of Aflatoxins in Grains
or Food Using Accelerated Solvent Extraction followed by HPLC
Fast and Effective Determination of Aflatoxins in Grains or Food Using Accelerated Solvent Extraction followed by HPLC

4.
Determination of Aflatoxins in Food Products by the ELISA Method
Determination of Aflatoxins in Food Products by the ELISA Method