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首页> 外文期刊>Chromatographia >A novel labeling reagent of 2-(12-benzo[b]acridin-5-(12H)-yl)- acetohydrazide for determination of saturated and unsaturated fatty acids in traditional Chinese herbs by HPLC-APCI-MS
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A novel labeling reagent of 2-(12-benzo[b]acridin-5-(12H)-yl)- acetohydrazide for determination of saturated and unsaturated fatty acids in traditional Chinese herbs by HPLC-APCI-MS

机译:新型标记试剂2-(12-苯并[b] ac啶-5-(12H)-基)-乙酰肼用于HPLC-APCI-MS测定中草药中的饱和和不饱和脂肪酸

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摘要

A new fluorescence labeling reagent 2-(12-benzo[b]acridin-5(12H)-yl)- acetohydrazide (BAAH) has been designed for fatty acids labeling. Eleven fatty acids containing seven saturated and four unsaturated fatty acids were used to evaluate the analytical potential of this reagent. The labeling reaction of BAAH with fatty acids was completed at 85 °C for 60 min using 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC·HCl) as the condensing agent. Separation of the derivatized fatty acids was carried out on a reversed-phase Thermo Hypersil Gold C18 column (4.6 mm × 250 mm, 5 μm) in combination with a gradient elution with a good baseline resolution. The fluorescence excitation and emission wavelengths were set at λ _(ex) 280 and λ _(em) 510 nm, respectively. The identification was carried out by the online APCI-MS in positive-ion detection mode. Linear correlation coefficients for all fatty acid derivatives were of >0.9994. Detection limits, at a signal-to-noise ratio of 3:1, were 3.89-12.5 nmol L -1 for the labeled fatty acids. The developed method was successfully applied to the accurate determination of fatty acids in five traditional Chinese herbs with satisfactory results.
机译:一种新的荧光标记试剂2-(12-苯并[b] ac啶-5(12H)-基)-乙酰肼(BAAH)已被设计用于脂肪酸标记。使用包含七个饱和和四个不饱和脂肪酸的十一个脂肪酸来评估该试剂的分析潜力。使用1-乙基-3-(3-二甲基氨基丙基)-碳二亚胺盐酸盐(EDC·HCl)作为缩合剂,BAAH与脂肪酸的标记反应在85°C下完成60分钟。衍生的脂肪酸的分离在反相Thermo Hypersil Gold C18色谱柱(4.6 mm×250 mm,5μm)上进行,同时具有良好的基线分辨率的梯度洗脱。荧光激发和发射波长分别设置为λ_(ex)280和λ_(em)510 nm。鉴定是通过在线APCI-MS在阳离子检测模式下进行的。所有脂肪酸衍生物的线性相关系数均大于0.9994。信噪比为3:1时,标记脂肪酸的检测限为3.89-12.5 nmol L -1。该方法成功用于五种中草药中脂肪酸的准确测定,结果令人满意。

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