浙贝母植株各部位中生物碱和黄酮的LC-LTQ-Orbitrap MS^n分析  

Identification of alkaloids and flavonoids in all parts of Fritillaria thunbergii using LC-LTQ-Orbitrap MS^n

作　　者：崔明超[1,2] 张加余[3] 陈少军[1] 江海龙 周海滨 凌庆枝[1] 

机构地区：[1]浙江医药高等专科学校,浙江宁波315100 [2]南京中医药大学,江苏南京210046 [3]北京中医药大学科研实验中心,北京100029 [4]宁波立华制药有限公司,浙江宁波315174

出　　处：《中国中药杂志》2016年第11期2124-2130,共7页China Journal of Chinese Materia Medica

基　　金：浙江省自然科学基金项目(LY15H28000);宁波市自然科学基金项目(2015A610290);鄞州区农业与社会发展科技项目(鄞科[2015]69号)

摘　　要：利用LC-LTQ-Orbitrap MS^n对浙贝母花、花蕾、茎、叶以及鳞茎中的生物碱和黄酮类成分进行鉴定。生物碱鉴定采用ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱,10 mmol·L^(-1)甲酸铵溶液-乙腈为流动相,梯度洗脱,正离子质谱检测模式;黄酮鉴定采用Agilent-Zorbax SB C18(4.6 mm×250 mm,5μm)色谱柱,0.2%乙酸-乙腈为流动相,负离子质谱检测模式。根据高分辨质谱提供的精确质量数和二级碎片离子信息,并结合文献报道,从浙贝母植株各部位中鉴定37个生物碱,主要包括7个生物碱(浙贝宁苷、贝母辛、贝母素甲、贝母素乙、去氢鄂贝啶碱或浙贝丙素、鄂贝啶碱或蒲贝素A、贝母辛氮氧化物)及同分异构体;同时鉴定了16个黄酮类成分,主要包括槲皮素、山柰酚及其苷。上述结果表明,浙贝母植株地上各部位与鳞茎所含的生物碱种类大致相同,且含有鳞茎中未检测到的黄酮类成分,具有一定的开发利用价值。Alkaloids and fiavonoids in flowers, flower buds, stems, leaves, and bulbs of Fritillaria thunbergii were identified by LC-LTQ-Orbitrap MS^n. Alkaloids were identified by ACQUITY UPLC BEH ClS （2. 1 mm × 50 mm, 1.7 μm ） chromatographic column with a mobile phase of 10 mmol . L ^-1 ammonium formate-acetonitrile and gradient elution in positive MS scan mode. Meanwhile, flavonoids were analyzed by Agilent-Zorbax SB C18 （4. 6 mm ×250 mm, 5 μm） chromatographic column with a mobile phase of 0. 2% acetic acid-acetonitrile and gradient elution in negative MS scan mode. Combined with literature reports, chemical constituents were identified and determined by accurate molecular weights and fragment ion peaks in the ESI-MS/MS spectra based on high resolution mass spectrometer. In all parts of F. thunbergii, 37 alkaloids including 7 alkaloids （ zhebeininoside, peimisine, peimine, peiminine, ebeiedinone/puqiedinone, ebeiedine/puqiedine, peimisine-N-oxide） were simultaneously analyzed. Moreover, 16 flavonoids including quercetin, kaempferol and their glycosides were identified. The results indicated that the aerial parts had the similar alkaloids as the bulbs on the whole. Meanwhile, it had a series of flavonoids undetected in the bulbs. Our results provided the scientific basis for the de velopment and utilization of aerial parts of F. thunbergii.

关 键 词：浙贝母 LC-LTQ-Orbitrap MSN 生物碱 黄酮 

分 类 号：R284.1[医药卫生—中药学]