论文部分内容阅读
目的:建立一种固相微萃取-高效液相色谱联用测定马钱子中士的宁、马钱子碱含量的新方法。方法:自制毛细管整体柱,用于固相微萃取-高效液相色谱联用在线测定马钱子中士的宁和马钱子碱含量。色谱柱为Hypersil ODS柱(150 mm×4.6 mm,5μm);以乙腈-0.01 mol·L~(-1)庚烷磺酸钠与0.02 mol·L~(-1)磷酸二氢钾等量混合溶液(用10%磷酸调节p H至2.8)(21∶79)为流动相;检测波长为260 nm,进样量为20μl,柱温为25℃。结果:士的宁在1.2~90.0μg·ml~(-1)(r=0.999 8)范围内,马钱子碱在1.0~75.0μg·ml~(-1)(r=0.999 6)范围内线性关系良好;平均回收率分别为100.05%(RSD=0.58%)、99.98%(RSD=0.27%)(n=6)。结论:该方法准确、高效,适用于马钱子中士的宁、马钱子碱含量的分析。
OBJECTIVE: To establish a new method for the determination of strychnine and strychnine in Strychnos nux vomica by solid-phase microextraction coupled with high performance liquid chromatography. Methods: Self - made monolithic capillary column was used for the determination of ning and brucine in Strychnos nux vomica on - line by solid phase microextraction coupled with high performance liquid chromatography. The column was Hypersil ODS column (150 mm × 4.6 mm, 5 μm). The mixture of acetonitrile-0.01 mol·L -1 heptane sulfonate and 0.02 mol·L -1 potassium dihydrogen phosphate The solution (adjusted to pH 2.8 with 10% phosphoric acid) (21:79) was used as the mobile phase. The detection wavelength was 260 nm and the injection volume was 20μl. The column temperature was 25 ℃. Results: In the range of 1.2 ~ 90.0μg · ml ~ (-1) (r = 0.999 8), strychnine was in the range of 1.0 ~ 75.0μg · ml ~ (-1) (r = 0.999 6) The linearity was good. The average recoveries were 100.05% (RSD = 0.58%) and 99.98% (RSD = 0.27%) (n = 6) respectively. Conclusion: This method is accurate and efficient and suitable for the determination of strychnine in strychnos.