Enhancement of atmospheric pressure chemical ionization for the determination of free and glycine-conjugated bile acids in human serum

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	Enhancement of atmospheric pressure chemical ionization for the determination of free and glycine-conjugated bile acids in human serum
	You, Jinmao ; Shi, Yunwei ; Zhao, Xianen ; Zhang, Haifeng ; Suo, Yourui ; Li, Yulin ; Wang, Honglun ; Sun, Jing
	2006-12-01
发表期刊	JOURNAL OF SEPARATION SCIENCE
卷号	29 期号:18 页码:2837-2846
文章类型	Article
摘要	A highly sensitive and accurate method based on the precolumn derivatization of bile acids (BA) with a high ionization efficiency labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl-benzenesulfonate (BDEBS) coupled with LC/MS has been developed. After derivatization, BA molecules introduced a weak basic nitrogen atom into the molecular core structure that was readily ionized in commonly used acidic HPLC mobile phases. Derivatives were sufficiently stable to be efficiently analyzed by atmospheric pressure chemical ionization (APCI)-MS/MS in positive-ion mode. The MS/MS spectra of BA derivatives showed an intense protonated molecular ion at m/z [M + H](+). The collision-induced dissociation of the molecular ion produced fragment ions at [MH - H2O](+), [MH - 2H(2)O](+), [MH - 3H(2)O](+). The characteristic fragment ions were at m/z 320.8, 262.8, and 243.7 corresponding to a cleavage of N - CO, O - CO, and C - OCC, respectively, and bonds of derivatized molecules. The selected reaction monitoring, based on the m/z [M + H]+ -> [MH - H2O](+), [MH - H2O](+), [MH - 2H(2)O](+), [MH-3H(2)O](+), 320.8, 262.8, and 243.7 transitions, was highly specific for the BA derivatives. The LODs for APCI in a positive-ion mode, at an S/N of 5, were 44.36-153.6 fmol. The validation results showed high accuracy in the range of 93-107% and the mean interday precision for all standards was < 15% at broad linear dynamic ranges (0.0244-25nmol/mL). Good linear responses were observed with coefficients of > 0.9935 in APCI/MS detection. Therefore, the facile BDEBS derivatization coupled with mass spectrometric analysis allowed the development of a highly sensitive and specific method for the quantitation of trace levels of the free and glycine-conjugated BA from human serum samples.; A highly sensitive and accurate method based on the precolumn derivatization of bile acids (BA) with a high ionization efficiency labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl-benzenesulfonate (BDEBS) coupled with LC/MS has been developed. After derivatization, BA molecules introduced a weak basic nitrogen atom into the molecular core structure that was readily ionized in commonly used acidic HPLC mobile phases. Derivatives were sufficiently stable to be efficiently analyzed by atmospheric pressure chemical ionization (APCI)-MS/MS in positive-ion mode. The MS/MS spectra of BA derivatives showed an intense protonated molecular ion at m/z [M + H](+). The collision-induced dissociation of the molecular ion produced fragment ions at [MH - H2O](+), [MH - 2H(2)O](+), [MH - 3H(2)O](+). The characteristic fragment ions were at m/z 320.8, 262.8, and 243.7 corresponding to a cleavage of N - CO, O - CO, and C - OCC, respectively, and bonds of derivatized molecules. The selected reaction monitoring, based on the m/z [M + H]+ -> [MH - H2O](+), [MH - H2O](+), [MH - 2H(2)O](+), [MH-3H(2)O](+), 320.8, 262.8, and 243.7 transitions, was highly specific for the BA derivatives. The LODs for APCI in a positive-ion mode, at an S/N of 5, were 44.36-153.6 fmol. The validation results showed high accuracy in the range of 93-107% and the mean interday precision for all standards was < 15% at broad linear dynamic ranges (0.0244-25nmol/mL). Good linear responses were observed with coefficients of > 0.9935 in APCI/MS detection. Therefore, the facile BDEBS derivatization coupled with mass spectrometric analysis allowed the development of a highly sensitive and specific method for the quantitation of trace levels of the free and glycine-conjugated BA from human serum samples.
关键词	Bile Acids 1 Derivatization 2-benzo-3 Human Serum 4-dihydrocarbazole-9-ethyl-benzenesulfonate Lc Ms
WOS标题词	Science & Technology ; Physical Sciences
学科领域	生物科学
关键词[WOS]	PERFORMANCE LIQUID-CHROMATOGRAPHY ; MASS-SPECTROMETRY ; FLUORESCENCE DETECTION ; GAS-CHROMATOGRAPHY ; BIOLOGICAL-FLUIDS ; SILICA CARTRIDGES ; REAGENT ; COLUMN ; DERIVATIZATION ; EXTRACTION
收录类别	SCI
语种	英语
WOS研究方向	Chemistry
WOS类目	Chemistry, Analytical
WOS记录号	WOS:000243338800017
引用统计	被引频次：16[WOS] [WOS记录] [WOS相关记录]
文献类型	期刊论文
条目标识符	http://210.75.249.4/handle/363003/1301
专题	中国科学院西北高原生物研究所
作者单位	1.Qufu Normal Univ, Coll Chem Sci, Shandong 273165, Peoples R China 2.Chinese Acad Sci, NW Plateau Inst Biol, Xining, Peoples R China
推荐引用方式 GB/T 7714	You, Jinmao,Shi, Yunwei,Zhao, Xianen,et al. Enhancement of atmospheric pressure chemical ionization for the determination of free and glycine-conjugated bile acids in human serum[J]. JOURNAL OF SEPARATION SCIENCE,2006,29(18):2837-2846.
APA	You, Jinmao.,Shi, Yunwei.,Zhao, Xianen.,Zhang, Haifeng.,Suo, Yourui.,...&Sun, Jing.(2006).Enhancement of atmospheric pressure chemical ionization for the determination of free and glycine-conjugated bile acids in human serum.JOURNAL OF SEPARATION SCIENCE,29(18),2837-2846.
MLA	You, Jinmao,et al."Enhancement of atmospheric pressure chemical ionization for the determination of free and glycine-conjugated bile acids in human serum".JOURNAL OF SEPARATION SCIENCE 29.18(2006):2837-2846.

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