LC-MS同时测定大型海藻中9个植物激素  

LC-MS simultaneous determination of nine phytohormones in macroalgaes

作　　者：刘雪梅[1] 赵鹏[1] 徐继林[1] 骆其君[1] 王秀娟[1] 陈海敏[1] 严小军[1] 

机构地区：[1]宁波大学应用海洋生物技术教育部重点实验室,宁波315211

出　　处：《药物分析杂志》2012年第10期1747-1752,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家科技支撑计划(2011BAD13B08);国家公益性行业(海洋)科研专项经费项目(201105009;201205029);国家公益性行业(农业)科研专项经费项目(201003068);浙江省公益性项目(2010C32021);浙江省自然科学基金(Y3100534)

摘　　要：目的:利用高效液相色谱-三重四极杆质谱(HPLC-QqQ MS)联用分析系统建立几种大型海藻中植物激素的分析方法。方法:冷冻干燥后的藻样用甲醇-水-甲酸(15∶4∶1,v/v/v)提取。9个中、酸性植物激素分别在Hypersil Gold C18色谱柱上实现分离,流动相为水(A)-甲醇(B),梯度洗脱,流速0.3 mL·min-1,柱温30℃。在电喷雾电离源正离子模式下,分别取m/z 130.0,204.1,136.1,220.0作为吲哚乙酸、异戊烯腺苷、异戊烯腺嘌呤和反式玉米素核苷的定量目标离子;在负离子模式下分别取153.3,91.3,93.2,143.2,59.5作为脱落酸、苯乙酸、水杨酸、赤霉素和茉莉酸的定量目标离子进行检测。结果:植物激素浓度在5～500μg·L-1范围内线性良好,检测限为0.0041～0.8622μg·L-1,回收率在61.33%～90.39%之间,RSD<11%(n=3)。结论:本法操作简单,准确可靠,适用于藻类植物激素的含量检测。Objective：To develop a method for the determination of phytohormones in several macroalgaes.Methods：The tissues were extracted with methanol-water-formic acid（15∶ 4∶ 1,v/v/v）.Nine kinds of phytohormones were separated with high efficiency in the selective reaction monitoring（SRM） mode on Hypersil Gold C18 column,with the mobile phase consisting of water（A） and methanol（B） in a programmed gradient elution.The flow rate was 0.3 mL·min-1 and the column temperature was 30 ℃.The mass spectrometry was performed using precursor ions at m/z 130.0,204.1,136.1 and 220.0 as quantitative ions in positive mode for indole-3-acetic acid,N6-（2-isopentyl） adenosine,N6-（2-isopentenyl） adenosine and trans-zeatin riboside,respectively.Meanwhile,in negative mode,m/z 153.3,91.3,93.2,143.2 and 59.5 were used as quantitative ions for abscisic acid,phenylacetic acid,salicylic acid,gibberellin A3 and jasmonic acid.Results：An excellent linear relationship was achieved in the range of 5-500 μg·L-1,detection limit of phytohormones was from 0.0041 μg·L-1 to 0.8622 μg·L-1,the recoveries varied between 61.33%-90.39% with RSD11%（n=3）.Conclusion：This method of the operation is accurate,reliable and can be used for the phytohormones content determination in macroalgaes.

关 键 词：大型海藻 植物激素 吲哚乙酸 异戊烯腺苷 异戊烯腺嘌呤 反式玉米素核苷 脱落酸 苯乙酸 水杨酸 赤霉素 茉莉酸 高效液相色谱-三重四极杆质谱 厚膜藻 角叉菜 石莼 浒苔 羊栖菜 鼠尾藻 

分 类 号：R917[医药卫生—药物分析学]