摘要
目的应用气相色谱-质谱联用(GC-MS)技术结合多元统计分析,筛选白木香叶中与沉香树脂形成相关的指标性成分。方法以GC-MS法分析已结香和未结香的白木香叶三氯甲烷提取物,正交偏最小二乘法判别分析(OPLS-DA)对样品进行分组,变量权重(VIP)结合相关系数[P(corr)]筛选差异组分,自动质谱退卷积定性系统(AMDIS)结合保留指数(RI)鉴定差异组分。以GC-MS的选择性离子检测(SIM)模式测定差异组分油酸酰胺、芥酸酰胺含量。结果已结香和未结香白木香叶中,与贮存时长无关的差异组分为油酰酸胺、芥酸酰胺、三十二烷、α-香树脂醇和羽扇豆醇。油酸酰胺和芥酸酰胺线性范围分别为0.68~6.8μg·mL^(-1)(r=0.9993)和2.72~27.2μg·mL^(-1)(r=0.9997);平均加样回收率分别为99.9%(RSD=3.69%)和93.8%(RSD=3.23%)。未结香组油酸酰胺与芥酸酰胺的平均含量均高于各结香组,而且未结香组油酸酰胺含量明显高于化学试剂诱导组(P<0.05)。结论油酰酸胺和芥酸酰胺可作为白木香叶中与贮存时长无关、与沉香树脂形成相关的指标性成分,可为沉香的采收时间提供判断依据。
Objective To screen the indicative components between the leaves of Aquilaria sinensis and resin involved in the formation of agarwood based on gas chromatography-mass spectrometry(GC-MS) combined with multivariate statistical analysis. Methods The chloroform extracts of the leaves from A. sinensis with or without resin were analyzed by GC-MS,and the samples were grouped by orthogonal partial least squares discriminant analysis(OPLS-DA). Variable importance in projection(VIP)combined with correlation coefficient [P(corr)] was used to screen the differential components. Automated mass spectral deconvolution and identification system(AMDIS)coupled with retention index(RI)were used to identify the differential components. The selected ion monitor(SIM)mode of GC-MS was used to determine the contents of oleamide and 13-docosenamide in the leaves of A. sinensis.Results The different components unrelated to the storage time in leaves from two kinds of A. sinensis were oleamide, 13-docosenamide, dotriacontane, α-amyrin, and lupeol. The calibration curves were linear over the ranges of 0.68-6.8 μg·mL^(-1)(r=0.999 3)and 2.72-27.2 μg·mL^(-1)(r=0.999 7)for oleamide and 13-docosenamide,respectively. The sample recovery rates of oleamide and 13-docosenamide were 99.9%(RSD=3.69%)and 93.8%(RSD=3.23%),respectively. The average contents of oleamide and 13-docosenamide in non-resinous group were higher than that in agarwood-producing group. The oleamide content in non-resinous group was significantly higher than that in chemical stimulation group(P<0.05). Conclusion Oleamide and 13-docosenamide can be used as indicative components between the leaves of non-resinous and agarwood-producing Aquilaria tree which were independent of storage time,which can provide basis for the harvest time of the resin of A. sinensis.
作者
孙雯霞
黄跃前
叶世楷
许凌雯
赵晶
刘小华
周欣
高晓霞
陈晓颖
SUN Wenxia;HUANG Yueqian;YE Shikai;XU Lingwen;ZHAO Jing;LIU Xiaohua;ZHOU Xin;GAO Xiaoxia;CHEN Xiaoying(School of Pharmacy,Guangdong Pharmaceutical University,Guangzhou 510006 Guangdong,China;Guangdong Yifang Pharmaceutical Co.Ltd.,Foshan 528244 Guangdong,China;Shimadzu(China)Co.Ltd.,Guangzhou 510656 Guangdong,China)
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2022年第4期512-521,共10页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
广东省科技计划项目(2017A020213014)
华南应用微生物国家重点实验室开放基金项目(SKLAM002-2018)
广东药科大学2020年省级大学生创新创业训练计划项目(202010573018)
广东省科技创新战略专项资金(“攀登计划”专项资金,pdjh2021b0265)。
关键词
白木香叶
气相色谱-质谱联用
多元统计分析
油酸酰胺
芥酸酰胺
含量测定
Leaves of Aquilaria sinensis
gas chromatography-mass spectrometry
multivariate statistical analysis
oleamide
13-docosenamide
quantitative determination