柱前衍生化-HPLC法同时测定注射用沙棘籽油中脂肪酸的含量Determination of the content of fatty acids in Hippophae rhamnoides L. seed oil by HPLC with precolumn derivatization
王晓丽,杨明明,迟娜,唐星
WANG Xiao-li,YANG Ming-ming,CHI Na,TANG Xing(School of Pharmacy
摘要(Abstract):
目的建立沙棘籽油中脂肪酸的HPLC测定法。方法以2,4′-二溴苯乙酮为衍生化试剂,18-冠醚-6为相转移催化剂,采用Kromasil C8反相色谱柱(250 mm×4.6 mm,5μm),检测波长254 nm,以甲醇-乙腈-水(体积比60∶30∶10)为流动相等度洗脱,柱温为室温,流速为1.0 mL.min-1。十七烷酸为内标,一次基线分离5种脂肪酸,建立注射用沙棘籽油的脂肪酸含量测定的方法。结果α-亚麻酸的线性范围为2.02~20.22 ng,相关系数为0.999 1;亚油酸的线性范围为2.90~20.90 ng,相关系数为0.999 1;棕榈酸的线性范围为1.27~12.67 ng,相关系数为0.999 0;油酸的线性范围为1.92~19.16 ng,相关系数为0.999 0;硬脂酸的线性范围为0.30~3.04 ng,相关系数为0.999 1。α-亚麻酸、亚油酸、棕榈酸、油酸、硬脂酸的平均回收率分别为106.07%、104.13%、100.81%、99.43%、95.62%,RSD分别为2.64%、2.42%、3.14%、1.18%、2.24%(n=9)。结论本方法重现性好,定量准确,可作为注射用沙棘籽油中脂肪酸测定的定量方法 ,用于沙棘籽油的质量控制。
Objective To develop a method for the determination of fatty acid in Hippophae rhamnoides L.seed oil for injection by precolumn derivation HPLC.Methods The fatty acids were derivatized with 2,4′-dibromoacetophenone as derivative and 18-crown-6 as catalyst.Kromasil C8 column(250 mm×4.6 mm,5 μm)was used,methanol-acetonitrile-water(V∶V∶V=60∶30∶10)was used as eluent and the internal standard was heptadecanoic acid.The detection wavelength was set at 254 nm.Column temperature was fixed at room temperature,and the flow rate was 1.0 mL·min-1.Results The standard curves of α-linolenic,linoleic,palmitic,oleic,and steraric acid were linear within the range of 2.02-20.22 ng,2.90-20.90 ng,1.27-12.67 ng,1.92-19.16 ng and 0.30-3.04 ng,respectively.The five fatty acid recoveries were 106.07%,104.13%,100.81%,99.43%,95.62% and the RSD were 2.64%,2.42%,3.14%,1.18%,2.24%,respectively.Conclusions Five fatty acids are separated within 40 min during a single run.The present method is reliable and relatively simple for the determination of fatty acid in Hippophae rhamnoides L.seed oil.
关键词(KeyWords):
沙棘籽油;脂肪酸;高效液相色谱法;气相-质谱联用;含量测定
Hippophae rhamnoides L.seed oil;fatty acid;HPLC;GC-MS;content determination
基金项目(Foundation): 国家科技支撑计划课题资助项目(2006BAI06A18-03)
作者(Author):
王晓丽,杨明明,迟娜,唐星
WANG Xiao-li,YANG Ming-ming,CHI Na,TANG Xing(School of Pharmacy
DOI: 10.14066/j.cnki.cn21-1349/r.2010.10.007
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