问题：请各位老师指点：双酚A中酚羟基的测定方法？
类型：求助 (悬赏分:3分)
提问：byqkitty
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版块：分析化学(wangsui,maqinghe,peiliang,)
信誉：94%
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时间：2006-03-29 18:41:03 编辑加入/取消收藏订制/取消短消息举报该贴

是这样的，我用双酚A和环氧乙烷合成了双酚A聚醚，想知道双酚A聚醚中有多少酚羟基没有加上环氧乙烷，不知道用什么方法可测出来，请高人指点。先谢了！

回复人：celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间：2006-03-30 08:06:27 编辑

1楼

你的问题中OH有以下可能:
1.乙二醇封端的OH
2.双酚A封端的酚OH
3.游离的双酚A的酚OH
你的问题是看有多少酚羟基没有加上环氧乙烷.那就是检测酚OH了.
建议:
1.GC法测定游离的双酚A的含量
2.也可以用1HNMR测定游离的双酚A的含量和封端双酚A的酚OH(用DMSO-d6做溶剂)酚OH的信号在7-9ppm范围.
3.将样品硅醚化,或将样品乙酰化(反应很好做的)测定1HNMR,可以定量的.
有困难可以与我联系.

回复人：byqkitty,▲ (乐观，自信，天真) 时间：2006-03-30 19:06:58 编辑	2楼
“GC法测定游离的双酚A的含量”具体方法是什么，能详细些吗？再谢！

回复人：celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间：2006-03-31 09:57:21 编辑

3楼

可以参照下面文献条件
[Determination of bisphenol A in foods using GC/MS]

Shokuhin Eiseigaku Zasshi. 2001 Apr;42(2):71-8.
An analytical method using GC/MS was developed for bisphenol A (BPA) in foods and BPA was determined in canned foods and fresh foods such as vegetables, fruit and meat. BPA was extracted with acetone from the samples and the extract was concentrated at under 40 degrees C in vacuo to afford an aqueous solution, which was washed with hexane after alkalization and extracted with 50% diethyl ether-hexane after acidification. Extracts were cleaned up on a PSA and/or a C18 cartridge column, and BPA was derivatized with heptafluorobutyric anhydride and determined by GC/MS (SIM). This method was applicable to the detection and determination of BPA residues in food samples at the level of 1 ng/g. Among canned foods, BPA was found in 6 corned beef, 1 chicken, 9 sweet corn and 3 bean samples at the levels of 17-602 ng/g, 212 ng/g, 2.3-75 ng/g and 3.5-26 ng/g, respectively. BPA was also detected in 1 retort soup and 1 retort pack product at the levels of 11 ng/g and 86 ng/g, respectively. As for dairy products, BPA was not detected in butter and milk. Among fresh foods, BPA was detected in 2 fish and 3 liver samples at the levels of trace (tr)-6.2 ng/g and tr-2.2 ng/g, respectively. In vegetables, fruits and chocolates, a trace level of BPA was detected in only 1 chocolate. Traces of BPA were also detected in 3 samples of 6 boxed lunches.

Liquid phase microextraction with in situ derivatization for measurement of bisphenol A in river water sample by gas chromatography-mass spectrometry.
1: J Chromatogr A. 2006 Mar 31;1110(1-2):1-5. Epub 2006 Feb 3.
A new method that involves liquid phase microextraction (LPME) with in situ derivatization and gas chromatography-mass spectrometry (GC-MS) is described for the determination of trace amounts of bisphenol A (BPA) in river water samples. The LPME conditions, such as the type of extraction solvent and the extraction time, are investigated. Then, the extract is directly injected into GC-MS. The detection limit and the quantification limit of BPA in river water sample are 2 and 10pgml(-1) (ppt), respectively. The calibration curve for BPA is linear with a correlation coefficient of >0.999 in the range of 10-10,000pgml(-1). The average recoveries of BPA in river water samples spiked with 100 and 1000pgml(-1) BPA are 104.1 (RSD: 8.9%) and 98.3 (RSD: 3.2%), respectively, with correction using the added surrogate standard, bisphenol A-(13)C(12). This simple, accurate, sensitive and selective analytical method may be applicable to the determination of trace amounts of BPA in liquid samples.

回复人：byqkitty,▲ (乐观，自信，天真) 时间：2006-04-01 07:49:58 编辑	4楼
已经打分了。

得分人：celan-2,

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