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氮化硼纳米片辅助基质固相分散微萃取-高效液相色谱-紫外检测-离子淌度四极杆飞行时间质谱联用测定莲心生物碱

Boron nitride nanosheet-assisted matrix solid-phase dispersion microextraction of alkaloids from lotus plumule by high-performance liquid chromatography coupled with ultraviolet detection and ion mobility quadrupole time-of-flight mass spectrometry.

机构信息

College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, P. R. China.

出版信息

Electrophoresis. 2022 Feb;43(4):581-589. doi: 10.1002/elps.202100286. Epub 2021 Nov 21.

DOI:10.1002/elps.202100286
PMID:34755364
Abstract

A boron nitride nanosheet (BNNS)-assisted matrix solid-phase dispersion method was established to microextract alkaloids from medicinal plants. The target compounds were identified by high-performance liquid chromatography coupled with ultraviolet detection and ion mobility quadrupole time-of-flight mass spectrometry. During the experimental process, several important parameters, including the type of dispersant, the amount of dispersant, the grinding time, and the type of elution solvent, were optimized. Finally, the BNNSs were chosen as the best dispersant, and their microcosmic morphologies were identified by scanning electron microscopy and transmission electron microscopy. Because of the special property of BNNSs, the cost of this experiment was greatly reduced, especially in elution volume, sample amount (50 mg), and extraction time (2 min). Under the best conditions, 50 mg of sample powder was dispersed with 50 mg of BNNSs, the grinding time was 120 s, the mixed powder was eluted with 200 μL of methanol, and good linearity (r  > 0.9993) and satisfactory recoveries (80-100%) were obtained. The inter- and intraday precisions were acceptable, with RSDs lower than 2.01 and 4.84%, respectively. The limits of detection ranged from 2.54 to 15.00 ng/mL, and the limits of quantitation were 8.47 to 50.00 ng/mL. The proposed method was successfully applied for the determination of liensinine, isoliensinine, and neferine in lotus plumule.

摘要

一种氮化硼纳米片(BNNS)辅助的基质固相分散法被建立用于从药用植物中微萃取生物碱。通过高效液相色谱-紫外检测-离子淌度四极杆飞行时间质谱联用对目标化合物进行了鉴定。在实验过程中,优化了几个重要参数,包括分散剂的类型、分散剂的用量、研磨时间和洗脱溶剂的类型。最后,选择 BNNS 作为最佳分散剂,并通过扫描电子显微镜和透射电子显微镜对其微观形貌进行了鉴定。由于 BNNS 的特殊性质,该实验的成本大大降低,特别是在洗脱体积、样品量(50mg)和提取时间(2min)方面。在最佳条件下,将 50mg 样品粉末与 50mg BNNS 分散,研磨时间为 120s,用 200μL 甲醇洗脱混合粉末,得到了良好的线性(r>0.9993)和令人满意的回收率(80-100%)。日内和日间精密度均良好,RSD 分别低于 2.01%和 4.84%。检测限范围为 2.54-15.00ng/mL,定量限为 8.47-50.00ng/mL。该方法成功应用于测定莲子心中的莲心碱、异莲心碱和荷叶碱。

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