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中国科学院上海原子核研究所
Received:06 June 1986,
Published:1987-08
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Liming Zhang. The quantitative determination of 13C palmitic acid using microsample technique of 13C NMR spectroscopy[J]. Nuclear techniques, 1987, 10(8): 39-40,62.
13
C核磁共振定量技术既可应用于
13
C标记化合物的结构定位,标记定量,又可间接应用于
13
C标记化合物的制备过程中。
J.N.Shoolery曾用
13
C核磁共振法测定植物油中脂肪酸组成
[1,2]
,但误差较大;后来关剑秋等人从样品的自旋—晶格弛豫时间(
T
1
)的缩短、核的NOE效应的消除及核磁共振参数设定等方面进行了进一步探讨
[3]
。我们采用微样品技术(
ф
1.7mm、C/H双探头、取样量为毫克级)测定
13
C标记正十六酸,可使灵敏度增加5倍左右。
The combined action of relexation reagent
chromium acetyl acetonate
with inversion gated control technique was studied and used to get a quantitative
13
C NMR spectra using microsample technique in the range of 3—5 mg. This method may be used as an alternative for obtaining
13
C labelled palmitic acid
which is a tracer for heart muscle studies. A good results have been obtained
in which
the enriched factor reached to 48 between C=O group at 175 ppm and - (CH)
10
at 29.7 ppm.
This means that
13
C isotope was enriched on C=0 group thus the same procedure may be applied to prepare
13
C labelled compounds.
J. N. Shoolery , Prog. NMR Spectroscopy , 11 , 79 ( 1977 ).
J. N. Shoolery and W. L. Budde , Anal. Chem. , 48 , 1158 ( 1976 ).
关剑秋 等 , 分析化学 , 12 , 6 , 484 ( 1984 )。
Sadtler Research Lab ., Sadtler standard cabon-13 NMR spectroscopy, S126, V21-24, 4604c , 1978 .
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