蒜氨酸光学纯度和立体构型的研究  

Study on the optical purity and configuration of alliin

作　　者：袁耀佐[1] 顾洁[1] 贺霞 杭太俊[1] 陈坚[3] 张正行[1] 

机构地区：[1]中国药科大学药物分析室 [2]伊犁州药品检验所,伊犁835000 [3]新疆医科大学药学院药分教研室,乌鲁木齐830054

出　　处：《药物分析杂志》2007年第10期1567-1571,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:研究国产蒜氨酸的光学纯度及其立体构型。方法:采用邻苯二甲醛/N-异丁酰基-L-半胱氨酸(OPA/IBLC)为柱前手性衍生化试剂,建立了柱前衍生化 RP-HPLC 法测定蒜氨酸的光学纯度,色谱条件为:SHIM-PACK CLC-ODS 柱(5μm,4.6mm×150mm),流动相为甲醇-醋酸盐缓冲液(1000 mL 水,加醋酸铵1 g 和冰醋酸1 mL)(50:50),UV/MS 检测,UV检测波长230 nm,MS 采用 SIM[M+H]^+m/z 467检测;流速1.0 mL·min^(-1),UV 检测限约为0.4μg·mL^(-1),MS 检测限约为0.04μg·mL^(-1),采用高效液相色谱制备蒜氨酸工作对照品,测定其比旋度,确定其立体构型。结果:手性衍生化柱前 RP-HPLC 测定结果表明国产蒜氨酸中无光学异构体存在,自制蒜氨酸对照品比旋度测定结果与文献报道值一致。结论:国产蒜氨酸中无手性对映体杂质,其立体构型为(+)S-烯丙基-L-半胱氨酸亚砜。Objective：To study optical purity and stereo structure of domestic alliin sample. Methods：Domestic al- liin sample was derivatized with ortho - phthalaldehyde/N - isobutyryl - L - cysteine （ OPA/IBLC ）, and analysis was carried out on a SHIM - PACK CLC - ODS column（5 μm,4. 6 mm × 150 mm） with a mixture of methanol - acetate buffer（ added 1 mL glacial acetic acid into 1000 mL 0. 1% ammonium acetate solution） （50：50） as mobile phase at a flow rate of 1 mL · min^-1 at 230 nm detector and MS detector （ SIM [M ＋ H] ^＋ m/z 467 ）, the limit of UV - detection was about 0. 4 μg·mL^-1, the limit of MS - detection was about 0. 04 μg · mL^-1, the specific rotation of alliin＇s working reference substance which was prepared by preparative HPLC was determinated. Results：No chromatographic peak of derivatives of alliin＇s optical isomer was found in the HPLC chromatograms detected by UV or MS/MS detectors and the specific rotation of alliin＇s working reference substance was consistent with the data in early literature. Conclusion：No optical isomer includes in allyl - L - cysteine sulfoxide. domestic alliin sample and it＇s configuration is（ ＋ ）S -allyl - L - cysteine sulfoxide.

关 键 词：蒜氨酸 光学纯度 立体构型 

分 类 号：R917[医药卫生—药物分析学]