固相萃取-高效液相色谱测定饲料中新橙皮苷二氢查耳酮和柚皮苷二氢查耳酮

doi:10.3724/SP.J.1123.2019.01006

摘要/Abstract

摘要：

建立了固相萃取-高效液相色谱检测饲料中新橙皮苷二氢查耳酮（NHDC）和柚皮苷二氢查耳酮（Naringin DC）的方法。采用纯甲醇溶液进行超声辅助萃取样品，经HLB固相萃取柱净化后在XB-C₁₈（150 mm×4.6 mm，5 μm）色谱柱上分离，用甲醇/水作为流动相进行梯度洗脱，光电二极管阵列检测器进行检测。结果表明，新橙皮苷二氢查耳酮和柚皮苷二氢查耳酮在0.2~49.0 mg/L范围内具有良好的线性关系，相关系数均>0.999，定量限分别为0.02和0.01 mg/kg。日内和日间精密度分别为0.7%~4.1%和0.9%~6.0%。方法的加标回收率为86.2%~105.0%，相对标准偏差（RSDs）为1.0%~6.3%（n=3）。该方法能有效降低饲料基体成分的干扰，灵敏度高，重现性好，适用于饲料中新橙皮苷二氢查耳酮和柚皮苷二氢查耳酮的定量检测。

关键词: 高效液相色谱法, 固相萃取, 饲料, 新橙皮苷二氢查耳酮, 柚皮苷二氢查耳酮

Abstract:

A new method was established for the determination of neohesperidin dihydrochalcone (NHDC) and naringin dihydrochalcone (Naringin DC) in feeds by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol and were purified on an HLB solid-phase extraction column. Chromatographic separation was achieved on an XB-C₁₈ column (150 mm×4.6 mm, 5 μm) by linear gradient elution using methanol/water as the mobile phase. The analytes were detected by the diode array detector (DAD). The results revealed a good linear correlation (r>0.999) between the peak areas and mass concentrations of dihydrochalcone sweeteners in the range of 0.2-49.0 mg/L. The limits of quantification (LOQs) of NHDC and Naringin DC were 0.02 and 0.01 mg/kg, respectively. Intra- and inter-day reproducibilities were 0.7%-4.1% and 0.9%-6.0%, respectively. The spiked recoveries for the samples and relative standard deviations (RSDs) were 86.2%-105.0% and 1.0%-6.3% (n=3), respectively. It is both sensitive and repeatable for the quantitative determination of neohesperidin dihydrochalcone and naringin dihydrochalcone in feeds, and thus, can be used to effectively reduce interference in feeds.

Key words: feeds, high performance liquid chromatography (HPLC), naringin dihydrochalcone (Naringin DC), neohesperidin dihydrochalcone (NHDC), solid phase extraction (SPE)

中图分类号:

O658

潘城, 胡朝阳, 任小英, 吴凌, 黄何何, 江凤玲, 谢勇, 邱秀玉. 固相萃取-高效液相色谱测定饲料中新橙皮苷二氢查耳酮和柚皮苷二氢查耳酮[J]. 色谱, 2019, 37(6): 649-654.

PAN Cheng, HU Chaoyang, REN Xiaoying, WU Ling, HUANG Hehe, JIANG Fengling, XIE Yong, QIU Xiuyu. Determination of neohesperidin dihydrochalcone and naringin dihydrochalcone in feeds by solid phase extraction-high performance liquid chromatography[J]. Chinese Journal of Chromatography, 2019, 37(6): 649-654.

参考文献

[1] Lei L, Huang B H, Lu Y J, et al. China Condiment, 2014, 39(12):41 雷琳, 黄宝华, 卢宇靖, 等. 中国调味品, 2014, 39(12):41
[2] Chen L, Liu C B, Zhang Q, et al. The Beverage Industry, 2016(1):53 陈良, 刘传滨, 张钦, 等. 饮料工业, 2016(1):53
[3] Wen H L, Ouyang Z Y, Hu X B, et al. China Condiment, 2008(10):70 温辉梁, 欧阳振宇, 胡晓波, 等. 中国调味品, 2008(10):70
[4] Li A P.[MS Dissertation]. Guangzhou:South China University of Technology, 2016 李爱平.[硕士学位论文]. 广州:华南理工大学, 2016
[5] Official Journal of the European Union. Commission Implementing Regulation (EU) 2015/264 of 18 February 2015 Concerning the Authorisation of Neohesperidine Dihydrochalcone as a Feed Additive for Sheep, Fish, Dogs, Calves and Certain Categories of Pigs. (2015-02-19)[2019-01-30]. http://eur-lex.europa.eu/legal-content/EN/TXT/?qid=1525779829805&uri=CELEX:32015R0264.pdf
[6] Ministry of Agriculture. No. 2625 Bulletin of Ministry of Agriculture of the People's Republic of China. (2017-12-25)[2019-01-30]. http://www.moa.gov.cn/nybgb/2018/201801/201801/t20180129_6135954.htm 农业部. 中华人民共和国农业部公告第2625号. (2017-12-25)[2019-01-30]. http://www.moa.gov.cn/nybgb/2018/201801/201801/t20180129_6135954.htm
[7] Zhang J, Cai H Q, Yang J, et al. Science and Technology Food Industry, 2017, 38(19):256 张剑, 蔡函青, 杨捷, 等. 食品工业科技, 2017, 38(19):256
[8] Wang Z D, Chen L, Wang Y. China Condiment, 2016, 41(11):135 王振东, 陈良, 王洋. 中国调味品, 2016, 41(11):135
[9] Zhang J, Liu H F. China Patent, CN105628818A. 2016-06-01 张娇, 刘惠芳. 中国专利, CN105628818A. 2016-06-01
[10] Deng H, Zhao H X, Dai Y, et al. Feed Review, 2014(8):52 邓虹, 赵华修, 代勇, 等. 饲料博览, 2014(8):52
[11] Xu G B, Yuan X H, Suo Z R, et al. Food Research and Development, 2010, 31(11):153 徐国波, 袁小红, 索志荣, 等. 食品研究与开发, 2010, 31(11):153
[12] Andrzej W, Josephine M C, Manuela B. J Chromatogr A, 2007, 1157:187
[13] Ling M, Hou L L, Wang F. China Patent, CN105572289A. 2016-05-11 凌满, 侯玲玲, 王芳. 中国专利, CN105628818A. 2016-05-11
[14] Romina S, Samantha F, Lowri S. Food Addit Contam A, 2014
[15] Ruan L P, Cai M, Ji W L, et al. Chinese Journal of Food Hygiene, 2013, 25(4):331 阮丽萍, 蔡梅, 吉文亮, 等. 中国食品卫生杂志, 2013, 25(4):331
[16] Liao Z B, Zhao B X, Li G X, et al. Pharmacy Today, 2015, 25(6):409 廖政邦, 赵博欣, 李国锋, 等. 今日药学, 2015, 25(6):409
[17] Lorenzo R A, Pena M T, Fernández P, et al. Food Control, 2015, 47:43
[18] Ordoñez E Y, Rodil R, Quintana J B, et al. Food Chem, 2015, 169:162
[19] Núnez M, Borrul F, Pocurull E, et al. J Chromatogr A, 2017, 1479:32
[20] Paula A, Francesc B, Eva P, et al. J Chromatogr A, 2015, 1393:106
[21] Edgar Y O, José B Q, Rosario R, et al. J Chromatogr A, 2012, 1256:197
[22] Pérez-Ruiz T, Martínez-Lozano C, Tomás V, et al. Chromatographia, 2000, 51(7):385
[23] Yang L X, Wang L, Li K J, et al. Anal Methods, 2014, 6:9410
[24] European Commission. EURL Evaluation Report on Analytical Methods Submitted in Connection with the Application for the Authorisation of a New Feed Additove According to Regulation (EC) No 1831/2003. (2011-04-14)[2019-01-30]. https://ec.europa.eu/jrc/en/eurl/feed-additives/evaluation-reports.pdf
[25] Xiao W, Wan Y W, Wu Y A, et al. China Feed, 2018(23):68 肖维, 万译文, 伍远安, 等. 中国饲料, 2018(23):68
[26] Fan Z C, Han Z, Guo W B, et al. Chinese Journal of Chromatography, 2017, 35(6):627 范志辰, 韩铮, 郭文博, 等. 色谱, 2017, 35(6):627
[27] Wei Y J, Feng M, Zhu Z Y, et al. Chinese Journal of Chromatography, 2017, 35(8):891 魏云计, 冯民, 朱臻怡, 等. 色谱, 2017, 35(8):891
[28] Liu F, Ren A S, Ge P, et al. Journal of Instrumental Analysis, 2018, 37(6):696 刘飞, 任安书, 葛萍, 等. 分析测试学报, 2018, 37(6):696