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Identification of anionic supramolecular complexes of sulfonamide receptors with Cl-, NO3-, Br-, and I- by APCI-MS.
Journal of the American Society for Mass Spectrometry ( IF 3.2 ) Pub Date : 2005-08-01 , DOI: 10.1016/j.jasms.2005.04.008
Konstantinos Kavallieratos 1 , Alberto J Sabucedo , Amanda T Pau , Johanna M Rodriguez
Affiliation  

As part of a mass spectrometric investigation of the binding properties of sulfonamide anion receptors, an atmospheric pressure chemical ionization mass spectrometric (APCI-MS) method involving direct infusion followed by thermal desorption was employed for identification of anionic supramolecular complexes in dichloromethane (CH2Cl2). Specifically, the dansylamide derivative of tris(2-aminoethyl)amine (tren) (1), the chiral 1,3-benzenesulfonamide derivatives of (1R,2S)-(+)-cis-1-amino-2-indanol (2), and (R)-(+)-bornylamine, (3), were shown to bind halide and nitrate ions in the presence of (n-Bu)4N+X- (X- = Cl-, NO3-, Br-, I-). Solutions of receptors and anions in CH2Cl2 were combined to form the anionic supramolecular complexes, which were subsequently introduced into the mass spectrometer via direct infusion followed by thermal desorption. The anionic supramolecular complexes [M + X]-, (M = 1-3, X- = Cl-, NO3-, Br-, I-) were observed in negative mode APCI-MS along with the deprotonated receptors [M - H]-. Full ionization energy of the APCI corona pin (4.5 kV) was necessary for obtaining mass spectra with the best signal-to-noise ratios.

中文翻译:

通过APCI-MS鉴定磺酰胺受体与Cl-,NO3-,Br-和I-的阴离子超分子复合物。

作为对磺酰胺阴离子受体结合特性进行质谱研究的一部分,采用了直接注入然后热脱附的大气压化学电离质谱(APCI-MS)方法来鉴定二氯甲烷(CH2Cl2)中的阴离子超分子配合物。具体而言,是三(2-氨基乙基)胺(tren)的丹磺酰胺衍生物(1),(1R,2S)-(+)-顺-1-氨基-2-茚满醇(2)的手性1,3-苯磺酰胺衍生物(2)。 )和(R)-(+)-冰片胺(3)在(n-Bu)4N + X-(X- = Cl-,NO3-,Br- , 一世-)。合并受体和阴离子在CH2Cl2中的溶液以形成阴离子超分子络合物,然后通过直接注入然后进行热脱附将其引入质谱仪。在负模式APCI-MS中观察到阴离子超分子复合物[M + X]-(M = 1-3,X- = Cl-,NO3-,Br-,I-)以及去质子化的受体[M-H ]-。要获得具有最佳信噪比的质谱图,必须使用APCI电晕针的完全电离能(4.5 kV)。
更新日期:2019-11-01
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