蚕沙中叶黄素和β-胡萝卜素的含量测定及提取条件优化  

Determination and Extraction Condition Optimization of Lutein andβ-Carotene in Silkworm Excrement

作　　者：郑倩倩 王小芳 路丽娟 张淼 宋莎 赵艳普 ZHENG Qian-qian;WANG Xiao-fang;LU Li-juan;ZHANG Miao;SONG Sha;ZHAO Yan-pu(Shijiazhuang Food and Drug Inspection Center,Shijiazhuang 050000,China)

机构地区：[1]石家庄市食品药品检验中心,河北石家庄050000

出　　处：《食品与药品》2022年第2期127-132,共6页Food and Drug

基　　金：河北省中医药管理局科研计划项目(编号:2020356)。

摘　　要：目的建立同时测定蚕沙中叶黄素、β-胡萝卜素含量的方法,并优化其提取条件。方法采用高效液相色谱法(HPLC),全程避光操作。色谱柱为Agilent 5 TC-C_(18)(2)(250 mm×4.6 mm,5μm),以甲醇(A)-乙腈(B)-二氯甲烷(C)-水(D)为流动相,梯度洗脱,切换检测波长(442,450 nm),柱温为40℃,进样量为10μl。以叶黄素、β-胡萝卜素含量为指标,采用L_(9)(3^(4))正交试验优化提取条件并进行含量测定。结果叶黄素、β-胡萝卜素分别在0.197~19.7μg、0.216~21.6μg范围内呈良好的线性关系,相关系数(r)均>0.9990,平均回收率分别为96.84%~101.71%and,98.01%~103.29%。最佳提取条件为:丙酮为溶剂,料液比1:50(g/ml),40℃下超声提取30 min。结论所建含量测定方法操作简便,准确度高,可用于蚕沙的质量控制。优化所得的提取条件稳定、可行。Objective To establish a method for the simultaneous determination of lutein andβ-carotene in silkworm excrement and optimize the extraction conditions.Method HPLC was adopted,and the whole process was protected from light.The chromatographic column was Agilent 5 TC-C_(18)(2)(250 mm×4.6 mm,5μm),using methanol(A)-acetonitrile(B)-dichloromethane(C)-water(D)as mobile phase of gradient elution.The detection wavelength was changed from 442 nm to 450 nm.The column temperature was 40℃,and the injection volume was 10μl.With the content of lutein andβ-carotene as indicators,the L_(9)(3^(4)) orthogonal test was used to optimize the extraction conditions and determine the content.Results Lutein andβ-carotene showed good linear relationships in the mass range of 0.197-19.7μg and 0.216-21.6μg,respectively,the correlation coefficients(r)were all above 0.9990,and the average recoveries were 96.84%-101.71%and 98.01%-103.29%,respectively.The best extraction conditions were as follows:acetone was used as solvent,the ratio of material to liquid was 1:50(g/ml),and the silkworm excrement was ultrasonically extracted by for 30 min at 40℃.Conclusion The established method is easy to operate,highly accurate,and can be used for quality control of silkworm excrement.

关 键 词：HPLC 蚕沙 叶黄素 Β-胡萝卜素 提取条件 正交试验 

分 类 号：R284.1[医药卫生—中药学]