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
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篇名: 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
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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-C18,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20 μL。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、0.903~14.442 μg(r≥ 0.999 6)范围内线性关系良好;检测限分别为0.009 9、0.003 5 μg,定量限分别为0.024 8、0.008 9 μg;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。
ABSTRACT: 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 20 μL. 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 0.903-14.442 μg (r≥0.999 6), respectively. The detection limits were 0.009 9 and 0.003 5 μg, and limits of quantitation were 0.024 8 and 0.008 9 μg, 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.
期刊: 2018年第29卷第21期
作者: 高荣凯,关亮俊,任海东,王敏,李琦,张宏桂
AUTHORS: GAO Rongkai,GUAN Liangjun,REN Haidong,WANG Min,LI Qi,ZHANG Honggui
关键字: 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
KEYWORDS: Seeds of Raphanus sativus; HPLC; Glucoraphanin; 4-methylsulfoyl-3-butenyl glucosinolate; Content determination; Producing areas
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