HPLC法同时测定莱菔子中萝卜硫苷和4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷的含量  

Simultaneous Determination of Glucoraphanin and 4-methylsulfoyl-3-butenyl Glucosinolate in the Seeds of Raphanus sativus by HPLC

作　　者：高荣凯[1] 关亮俊 任海东 王敏[1] 李琦[1] 张宏桂[1] GAO Rongkai;GUAN Liangjun;REN Haidong;WANG Min;LI Qi;ZHANG Honggui(School of Chinese Materia Medica,Beijing University of TCM,Beijing 102488,China)

机构地区：[1]北京中医药大学中药学院,北京102488

出　　处：《中国药房》2018年第21期2898-2901,共4页China Pharmacy

基　　金：国家自然科学基金资助项目(No.31070328)

摘　　要：目的:建立同时测定莱菔子中萝卜硫苷和4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷含量的方法。方法:采用高效液相色谱法。色谱柱为Welch Ultimate LP-C_(18),流动相为甲醇-0.05 mol/L磷酸二氢钾溶液(梯度洗脱),流速为1.0 mL/min,检测波长为235 nm,柱温为30℃,进样量为20μL。采用建立的方法测定5个产地共15批样品中萝卜硫苷和4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷的含量。结果:萝卜硫苷、4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷进样量分别在0.248～3.960、0.903～14.442μg(r≥0.999 6)范围内线性关系良好;检测限分别为0.009 9、0.003 5μg,定量限分别为0.024 8、0.008 9μg;精密度、稳定性(24 h)、重复性试验的RSD均<2%(n=6);平均回收率分别为99.83%、100.40%(RSD分别为1.42%、1.50%,n=6)。在安徽、甘肃、河北、山东、云南5个产地共15批的莱菔子中,萝卜硫苷的平均含量分别为1.881、5.120、3.634、3.237、2.856 mg/g(n=3);4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷的平均含量分别为37.561、46.389、40.136、37.000、41.101 mg/g(n=3)。结论:所建立的含量测定方法简便、准确、重现性好,可用于莱菔子中萝卜硫苷和4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷含量的同时测定;5个产地莱菔子样品中萝卜硫苷和4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷的平均含量均以甘肃产最高。OBJECTIVE:To establish a method for simultaneous determination of glucoraphanin and 4-methylsulfoyl-3-butenyl glucosinolate in the seeds of Raphanus sativus.METHODS:HPLC was adopted.The determination was performed on Welch Ultimate LP-C18 column with mobile phase consisted of methanol-0.05 mol/L monobasic potassium phosphate(gradient elution)at the flow rate of 1.0 mL/min.The detection wavelength was set at 235 nm,and column temperature was 30℃.The sample size was 20μL.The established method was used to determine the contents of glucoraphanin and 4-methylsulfoyl-3-butenyl glucosinolate in 15 batches of samples from 5 producing areas.RESULTS:The linear range of glucoraphanin and 4-methylsulfoyl-3-butenyl glucosinolate were 0.248-3.960 and 0.903-14.442μg(r≥0.999 6),respectively.The detection limits were 0.009 9 and 0.003 5μg,and limits of quantitation were 0.024 8 and 0.008 9μg,respectively.RSDs of precision,stability(24 h)and reproducibility tests were all lower than 2%(n=6).The average recoveries were 99.83%and 100.40%(RSD=1.42%,1.50%,n=6).The average contents of 15 batches of glucoraphenin in the seeds of R.sativus from producing areas(Anhui,Gansu,Hebei,Shandong,Yunnan)were 1.881,5.120,3.634,3.237 and 2.856 mg/g(n=3).Average contents of 4-methylsulfoyl-3-butenyl glucosinolate were 37.561,46.389,40.136,37.000,41.101 mg/g(n=3).CONCLUSIONS:The established method is simple,accurate and repeatable,which can be used for content determination of glucoraphanin and 4-methylsulfoyl-3-butenyl glucosinolate in the seeds of R.sativus.Among samples of 5 producing areas,average contents of glucoraphanin and 4-methylsulfoyl-3-butenyl glucosinolate in the seed of R.sativus from Gansu province are the highest.

关 键 词：莱菔子 高效液相色谱法 萝卜硫苷 4-甲基亚磺酰基-3-丁烯基硫代葡萄糖苷 含量测定 产地 

分 类 号：R917[医药卫生—药物分析学] R284.1[医药卫生—药学]