|
|
Detection of Content and Isotope Abundance of 15N-S-benzyl-L-cysteine |
SONG Ming-ming;DU Xiao-ning |
Shanghai Research Institute of Chemical Industry, Shanghai 200062, China |
|
|
Abstract A HPLC method for determination of S-benzyl-L-cysteine in fermentation broth was established. Cosmosil C18 column(5 μm,150 mm×4.6 mm) was used with 2,4-dinitrofluorobenzene as derivatization reagent and 0.05 mol/L sodium acetate buffer (pH=6.5,including 10 mL/L N,N-dimethylformamide) and V(acetonitrile)∶V(water)=3∶1 as mobile phase. The content was detected at a flow rate of 1.0 mL/min(gradient), the detection wavelength was 350 nm, column temperature was 30 ℃. The calibration curves were linear in the range of 0.2~1.0 g/L(R2=0.998 6), the average recovery rates were 97.30%, the minimum limit was 3.95×10-4 g/L, the relative standard deviation of results was 0.55%. Microscale high temperature combustion-MS method was also described to detect the isotope abundance of 15N-SBC. The minimum consumption of 15N-SBC product was 2 mg, the optimal combustion temperature was 530 ℃ and reaction time was 3 h. The RSD of results was 0.17%.
|
Received: 01 January 1900
|
|
|
|
[1] |
孟献梁,荀志金,贺忠,等.硫代苄基半胱氨酸结晶介稳区的测定及分析[J].南京工业大学学报,2003,25(6):66-69.
|
[2] |
陈维一,陆军,蒋虹,等.含硫手性β-氨基醇的合成及其在对映选择还原反应中的应用[J].有机化学,2003, 23(12): 1 393-1 395.
|
[3] |
柯昌武,罗勇,潘洁,等.酶法拆分氮-15 标记S-苄基-半胱氨酸的研究[J].上海化工,2009,34(10):7-11.
|
[4] |
蔡东联,陈小莉.高效液相测定同型半胱氨酸方法的建立[J].氨基酸和生物资源,2001,23(1):48-51.
|
[5] |
Smith CS, Chalk PM. Nitrogen gas preparative system for isotope-ratio analysis by mass spectrometry[J]. Anal Chem Acta, 1979, 104: 245-252
|
[6] |
杜晓宁,宋明鸣,赵诚.质谱检测用同位素15N标记样品的处理方法[J].原子能科学技术,2009,43(增刊):59-63.
|
[7] |
杜晓宁,李良君,李虎林,等.HG/T 3789—2005 稳定性同位素氖气[S].北京:化学工业出版社,2005.
|
[8] |
杜晓宁,宋明鸣,赵诚,等. 13C-尿素同位素丰度的检测方法[J].同位素,2010,23(1):39-43.
|
|
|
|