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用密度测定 TLC 分析法控制枸杞中的莨菪烷和甾体生物碱。

Densitometric TLC analysis for the control of tropane and steroidal alkaloids in Lycium barbarum.

机构信息

Chair and Department of Pharmacognosy, Faculty of Pharmacy, Medical University of Gdansk, Hallera 107, 80-416 Gdansk, Poland.

Chair and Department of Pharmacognosy, Faculty of Pharmacy, Medical University of Gdansk, Hallera 107, 80-416 Gdansk, Poland.

出版信息

Food Chem. 2017 Apr 15;221:535-540. doi: 10.1016/j.foodchem.2016.11.142. Epub 2016 Nov 28.

Abstract

Thin layer chromatographic methods for quantitative determination of nightshade-specific tropane (l-hyoscyamine, scopolamine) and steroidal alkaloids (α-solanine, α-chaconine) in goji berries (L. barbarum L., Solanaceae) were developed. The analysis of tropane derivatives included separation on silica gel-coated HPTLC plates using mobile phase consisted of chloroform:methanol:acetone:25% ammonium hydroxide (75:15:10:1.6 v/v/v/v), derivatization with Dragendorff reagent and scanning densitometry at λ - 520nm in reflectance/absorption mode. Steroidal alkaloid analysis employed silica gel-coated TLC plates, mobile phase composed of chloroform:methanol:water:25% ammonium hydroxide (70:30:4:2 v/v/v/v), derivatization with Carr-Price reagent and video densitometry under white light in the reflectance mode. Both methods were validated with respect to linearity, precision, accuracy and sensitivity, enabling reliable detection of tropane derivatives and α-solanine at 1.20 and 7.84mgper100g fresh material, respectively. None of the analyzed compounds were detected in fruits, leaves, stems and roots of three L. barbarum varieties ('No. 1', 'New Big' and 'Amber Sweet Goji').

摘要

建立了薄层色谱法用于定量测定枸杞(茄科枸杞属)中茄科特有的托烷类生物碱(L-莨菪碱、东莨菪碱)和甾体生物碱(α-茄碱、α-卡茄碱)。托烷类衍生物的分析包括在硅胶涂覆的 HPTLC 板上进行分离,使用的流动相由氯仿:甲醇:丙酮:25%氨水溶液(75:15:10:1.6v/v/v/v)组成,用 Dragendorff 试剂衍生化,并在反射/吸收模式下在 λ-520nm 处扫描比色。甾体生物碱分析采用硅胶涂覆 TLC 板,流动相由氯仿:甲醇:水:25%氨水溶液(70:30:4:2v/v/v/v)组成,用 Carr-Price 试剂衍生化,并在白光反射模式下进行视频比色。这两种方法均进行了线性、精密度、准确度和灵敏度验证,能够可靠地检测托烷类衍生物和α-茄碱,其在 100g 新鲜材料中的检出限分别为 1.20 和 7.84mg。在三个枸杞品种('1 号'、'新大'和'琥珀甜枸杞')的果实、叶片、茎和根中均未检测到分析化合物。

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