暨南大学学报(自然科学与医学版)
暨南大學學報(自然科學與醫學版)
기남대학학보(자연과학여의학판)
JOURNAL OF JINAN UNIVERSITY(NATURAL SCIENCE & MEDICINE EDITION)
2014年
6期
519-524
,共6页
孙小慧%田海妍%闫研%殷果%王铁杰%江仁望
孫小慧%田海妍%閆研%慇果%王鐵傑%江仁望
손소혜%전해연%염연%은과%왕철걸%강인망
鸦胆子油%GC%β-谷甾醇%含量测定
鴉膽子油%GC%β-穀甾醇%含量測定
아담자유%GC%β-곡치순%함량측정
Bruceae Fructus oil%GC%β-sitosterol%content determination
采用溶剂提取和两次硅胶柱层析法分离鸦胆子油中的β-谷甾醇,并用波谱学方法进行鉴定;对鸦胆子油用氢氧化钾-乙醇皂化后,采用气相色谱法对β-谷甾醇的含量进行测定.色谱条件为:Agilent HP-5毛细管柱(30 m ×250μm ×0.25μm);FID 检测器;进样口温度为285℃;程序升温:270℃(24 min),10℃·min -1升温至280℃(15 min);检测器温度为300℃;分流比为40∶1;流速为1 mL·min -1;进样量为1μL.β-谷甾醇对照品的峰面积与质量浓度在0.02847~0.4100 mg·mL -1呈良好的线性关系(r =0.9994).该方法的平均回收率为95.2%(RSD =2.98%),测得8份样品中β-谷甾醇的质量分数在2.96~4.37 mg·g -1.本方法快速、简便、重复性好,可用于鸦胆子油中β-谷甾醇的含量测定.
採用溶劑提取和兩次硅膠柱層析法分離鴉膽子油中的β-穀甾醇,併用波譜學方法進行鑒定;對鴉膽子油用氫氧化鉀-乙醇皂化後,採用氣相色譜法對β-穀甾醇的含量進行測定.色譜條件為:Agilent HP-5毛細管柱(30 m ×250μm ×0.25μm);FID 檢測器;進樣口溫度為285℃;程序升溫:270℃(24 min),10℃·min -1升溫至280℃(15 min);檢測器溫度為300℃;分流比為40∶1;流速為1 mL·min -1;進樣量為1μL.β-穀甾醇對照品的峰麵積與質量濃度在0.02847~0.4100 mg·mL -1呈良好的線性關繫(r =0.9994).該方法的平均迴收率為95.2%(RSD =2.98%),測得8份樣品中β-穀甾醇的質量分數在2.96~4.37 mg·g -1.本方法快速、簡便、重複性好,可用于鴉膽子油中β-穀甾醇的含量測定.
채용용제제취화량차규효주층석법분리아담자유중적β-곡치순,병용파보학방법진행감정;대아담자유용경양화갑-을순조화후,채용기상색보법대β-곡치순적함량진행측정.색보조건위:Agilent HP-5모세관주(30 m ×250μm ×0.25μm);FID 검측기;진양구온도위285℃;정서승온:270℃(24 min),10℃·min -1승온지280℃(15 min);검측기온도위300℃;분류비위40∶1;류속위1 mL·min -1;진양량위1μL.β-곡치순대조품적봉면적여질량농도재0.02847~0.4100 mg·mL -1정량호적선성관계(r =0.9994).해방법적평균회수솔위95.2%(RSD =2.98%),측득8빈양품중β-곡치순적질량분수재2.96~4.37 mg·g -1.본방법쾌속、간편、중복성호,가용우아담자유중β-곡치순적함량측정.
The β-sitosterol was isolated by solvent extraction and silica gel column chromatography (two times),and identified by spectroscopic methods.A gas chromatography (GC)method was estab-lished for the determination of β-sitosterol in 8 batches of Bruceae Fructus oil.The oil samples of Bruceae Fructus from 8 different areas were analyzed by a Agilent HP-5 capillary column after saponification with KOH-EtOH.The temperature was maintained at 270 ℃ for 24 min,then increased to 280 ℃ at a rate of 10 ℃ ·min -1 and was maintained for 15 min.The injection temperature was 285 ℃ and the detection temperature was 300 ℃.Carrier gas was nitrogen,flow rate was 1.01 mL·min -1 with the spilt 40∶1. The linear range of β-sitosterol was 0.028 47 -0.410 0 mg·mL -1 (r =0.999 4).The average recovery was 95.2% (RSD =2.98%),and the content of β-sitosterol in 8 batches of Bruceae Fructus oil was in the range of 2.96 -4.37 mg·g -1 .The method for determining the content of β-sitosterol was accurate with good reproducibility,and could be used for the determination of β-sitosterol in Bruceae Fructus oil.