摘要
建立降香药材所含挥发油相对密度及反式苦橙油醇含量测定方法,并对不同商品来源降香药材进行质量评价。水蒸气蒸馏法提取降香挥发油,采用比重瓶法测定相对密度,气相色谱法测定反式苦橙油醇含量,采用HP-5色谱柱,FID检测器,以正十四烷为内标进行测定。比重瓶法准确性[RAD(相对平均偏差)%〈5%(n=10)]、重复性(RSD 0.04%〈2%)、中间精密度[RAD%〈5%(n=15)]均良好,可替代韦氏比重秤法(用量100 mL)用于降香药材相对密度检测。气相色谱法进样精密度RSD%=0.2%,重复性RSD%=0.5%,稳定性RSD%=0.6%,线性范围为0.203~5.080 mg/mL(r=0.9995),回收率为100.5%,RSD%=1.37%(n=6)。采用比重称法测定降香药材相对密度,供试品用量少(5 mL),方法简便可行,气相色谱法简单、灵敏、准确、重线性好,适用于降香油中反式苦橙油醇含量的测定,不同商品来源降香药材出油率、相对密度、反式苦橙油醇含量差别较大,分别为1.72%~3.50%、0.8680~0.9294/20℃、40.4%~85.4%。
The objectives of this study were to develop an analytical method for the determination of the relative density of volatile oil and concentration of d-nerolidol in Dalbergia odorifera, and hence to evaluate the quality of D. ododfera from different origins. D. odorifera volatile oll was extracted by steam distillation. The relative density of volatile oil was determined by pycnometer method. Gas chromatography coupled with flame ionization detector (GC-FID) was used to determine the concentration of d-nerolidol. Pycnometer method was accurate C RAD 〈5% ( n = 10 ) ] with good repeat- ability (RSD 0.04% 〈2% ) and precision [RAD% 〈5% (n = 15) ]. Westphal balance method was succeasfu]]y sub- stituted by pyenometer method to determinate the relative density of volatile oil in D. odorifera. C,C-FID method was ac- curate and precise with RSD% 〈 1%. The linear relationship within the range of 0.203 -5. 080 mg/mL(r =0. 9995) was good. The recovery was 100.5% with RSD 1.37% (n =6). Pycnometer method was simple for the determination of the relative density of volatile oil from D. odorifera with using less amount of sample. The developed C,C-FID method was accurate and sensitive with good reproducibility. This method was capable to be used for the determination of volatile oil in D. odorifera. The yield of volatile oil,relative density and concentration of d-nero]idol of volatile oil from D. odorifera varied with origins.
出处
《天然产物研究与开发》
CAS
CSCD
北大核心
2014年第10期1628-1633,共6页
Natural Product Research and Development
关键词
降香
比重瓶法
相对密度
气相色谱法
反式苦橙油醇
Dalbergia odorifera
pycnometer method
relative density
gas chromatography
d-nerolidol