研究论文 RESEARCH PAPER

宠物饲料中8种水溶性维生素同步分析方法研究

  • 严华 ,
  • 李兰 ,
  • 王继彤 ,
  • 贾铮 ,
  • 姚婷 ,
  • 刘佳 ,
  • 徐思远 ,
  • 田静 ,
  • 樊霞
展开
  • 1. 中国农业科学院农业质量标准与检测技术研究所, 北京 100081;
    2. 北京市兽药饲料监测中心, 北京 102200
严华(1978—),女,重庆人,副研究员,博士,主要从事饲料质量安全检测技术研究。E-mail:56431978@qq.com

收稿日期: 2022-05-31

  网络出版日期: 2022-12-15

基金资助

“十三五”国家重点研发计划项目课题(2019YFE0103800)

Simultaneous Analysis of 8 Water Soluble Vitamins in Pet Feed

  • YAN Hua ,
  • LI Lan ,
  • WANG Jitong ,
  • JIA Zheng ,
  • YAO Ting ,
  • LIU Jia ,
  • XU Siyuan ,
  • TIAN Jing ,
  • FAN Xia
Expand
  • 1. Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China;
    2. Beijing Veterinary Drug and Feed Monitoring Center, Beijing 102200, China

Received date: 2022-05-31

  Online published: 2022-12-15

摘要

本研究旨在建立宠物配合饲料中8种水溶性维生素(维生素B1、维生素B2、维生素B6、烟酸、烟酰胺、D-泛酸、D-生物素和叶酸)的同步分析方法。试验在宠物配合饲料样品中加入同位素内标,用1%盐酸溶液在50℃水浴40 min后,再用10%氨水溶液调节pH至6.0,沉淀后取上清液进行分析。以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相,SB-AQ C18色谱柱(100 mm×3.0 mm,1.8 μm)为分离柱,梯度洗脱,洗脱液经电喷雾离子源在正离子模式下进行电离,多反应监测模式采集数据,内标法定量。结果表明:8种水溶性维生素在5.0~2 000 ng/mL内具有良好的线性关系,相关系数(R2)大于0.995 0,犬粮和猫粮在3个添加水平下的加标回收率分别为80.0%~117.3%和81.0%~112.2%,相对标准偏差分别为1.04%~5.28%和1.06%~10.20%。该方法操作简便、过程快速、分析灵敏、结果准确,可实现宠物配合饲料中8种水溶性维生素的同时检测。

本文引用格式

严华 , 李兰 , 王继彤 , 贾铮 , 姚婷 , 刘佳 , 徐思远 , 田静 , 樊霞 . 宠物饲料中8种水溶性维生素同步分析方法研究[J]. 动物营养学报, 2022 , 34(12) : 8072 -8085 . DOI: 10.3969/j.issn.1006-267x.2022.12.054

Abstract

The aim of this study was to establish a method for the simultaneous analysis of 8 water soluble vitamins (vitamin B1, vitamin B2, vitamin B6, niacin, nicotinamide, D-pantothenic acid, D-biotin and folic acid) in pet compound feed. In the experiment, the isotope internal standard was added to the pet compound feed samples, the samples were water bathed 40 min at 50℃ with 1% hydrochloric acid solution and the pH of the solutions were then adjusted to 6.0 by 10% ammonia solution. After precipitation, the supernatant was taken for analysis. The 0.1% formic acid aqueous solution and 0.1% formic acid acetonitrile solution were used as mobile phase, SB-AQ C18 chromatographic column (100 mm×3.0 mm, 1.8 μm) was used as the separation column, and gradient elution was performed. The eluate was ionized by electrospray ion source in positive ion mode, and the data were collected in multiple reaction monitoring mode, and quantified by internal standard method. The results showed that the eight water soluble vitamins had a good linear relationship in the range of 5.0 to 2 000 ng/mL, and the correlation coefficient (R2) was greater than 0.995 0. The recovery rates of dog food and cat food were 80.0% to 117.3% and 81.0% to 112.2%, respectively, and the relative standard deviations were 1.04% to 5.28% and 1.06% to 10.20%, respectively. The method is simple, rapid, sensitive and accurate, and can be used for the simultaneous detection of 8 water soluble vitamins in pet compound feed.

参考文献

[1] 中国饲料工业协会.2021年全国饲料工业发展概况[EB/OL].(2022-02-11)[2022-05-10].http://www.nahs.org.cn/dt/xwlb/202202/t20220211_397140.htm. China Feed Industry Association.Overview of National Feed Industry Development in 2021[EB/OL].(2022-02-11)[2022-05-10].http://www.nahs.org.cn/dt/xwlb/202202/t20220211_397140.htm.(in Chinese).
[2] 国家市场监督管理总局, 国家标准化管理委员会.饲料中维生素B1的测定:GB/T 14700-2018[S].北京:中国标准出版社, 2018. State Administration for Market Regulation, Standardization Administration of the People's Republic of China.Determination of thiamine in feed:GB/T 14700-2018[S].Beijing:Standards Press of China, 2018.(in Chinese)
[3] 国家市场监督管理总局, 国家标准化管理委员会.饲料中维生素B2的测定:GB/T 14701-2019[S].北京:中国标准出版社, 2019. State Administration for Market Regulation, Standardization Administration of the People's Republic of China.Determination of vitamin B2 in feeds:GB/T 14701-2019[S].Beijing:Standards Press of China, 2019.(in Chinese)
[4] 中华人民共和国农业部.饲料中烟酰胺的测定 高效液相色谱法:NY/T 2130-2012[S].北京:中国农业出版社, 2012. Ministry of Agriculture of the People's Republic of China.Determination of niacinamide in feeds-high-performance liquid chromatography:NY/T 2130-2012[S].Beijing:Agriculture Press of China, 2012.(in Chinese)
[5] 中华人民共和国农业部.饲料中叶酸的测定 高效液相色谱法:NY/T 2895-2016[S].北京:中国标准出版社, 2016. Ministry of Agriculture of the People's Republic of China.Determination of folic acid in feeds-high-performance liquid chromatography:NY/T 2895-2016[S].Beijing:Agriculture Press of China, 2016.(in Chinese)
[6] 国家市场监督管理总局, 国家标准化管理委员会.添加剂预混合饲料中烟酸与叶酸的测定 高效液相色谱法:GB/T 17813-2018[S].北京:中国标准出版社, 2018. State Administration for Market Regulation, Standardization Administration of the People's Republic of China.Determination of niacin acid and folic acid in premix-high performance liquid chromatography:GB/T 17813-2018[S].Beijing:Standards Press of China, 2018.(in Chinese)
[7] 国家市场监督管理总局, 国家标准化管理委员会.添加剂预混合饲料中维生素B6的测定 高效液相色谱法:GB/T 14702-2018[S].北京:中国标准出版社, 2018. State Administration for Market Regulation, Standardization Administration of the People's Republic of China.Determination of vitamin B6 in premix-high performance liquid chromatography:GB/T 14702-2018[S].Beijing:Standards Press of China, 2018.(in Chinese)
[8] 中华人民共和国国家质量监督检验检疫总局, 中国国家标准化管理委员会.添加剂预混合饲料中维生素B12的测定 高效液相色谱法:GB/T 17819-2017[S].北京:中国标准出版社, 2017. Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China.Determination of vitamin B12 in additive premix-high performance liquid chromatography:GB/T 17819-2017[S].Beijing:Standards Press of China, 2017.(in Chinese)
[9] 中华人民共和国国家质量监督检验检疫总局, 中国国家标准化管理委员会.预混合饲料中泛酸的测定 高效液相色谱法:GB/T 18397-2014[S].北京:中国标准出版社, 2014. Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China.Determination of pantothenic acid in premix-high performance liquid chromatography:GB/T 18397-2014[S].Beijing:Standards Press of China, 2014.(in Chinese)
[10] 中华人民共和国国家质量监督检验检疫总局, 中国国家标准化管理委员会.预混合饲料中D-生物素的测定:GB/T 17778-2005[S].北京:中国标准出版社, 2005. Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China.Determination of D-biotin in premix:GB/T 17778-2005[S].Beijing:Standards Press of China, 2005.(in Chinese)
[11] HUANG L, TIAN S L, ZHAO W H, et al.Electrochemical vitamin sensors:a critical review[J].Talanta, 2021, 222:121645.
[12] FATIMA Z, JIN X Z, ZOU Y L, et al.Recent trends in analytical methods for water-soluble vitamins[J].Journal of Chromatography A, 2019, 1606:360245.
[13] 梁琳, 王英.HPLC法同步测定维生素预混合饲料中5种B族维生素[J].中国饲料, 2016(1):21-23, 38. LIANG L, WANG Y.The simultaneous determination of five vitamins B in vitamin premixes by a high performance liquid chromatography[J].China Feed, 2016(1):21-23, 38.(in Chinese)
[14] 张憬, 梁斌, 吴志奇, 等.高效液相色谱法同步测定添加剂预混合饲料中六种水溶性维生素[J].中国饲料, 2018(19):85-87. ZHANG J, LIANG B, WU Z Q, et al.Determining 6 kinds of water soluble vitamins in premixed feed additives by HPLC[J].China Feed, 2018(19):85-87.(in Chinese)
[15] FORGHIERI F, FORMISANO B, CASARIN L, et al."Fit-for-Purpose" simultaneous extraction of water-soluble vitamins (PP, B2, B6, B9, B5) from mineral feeds and premixes and simultaneous determination of B1 and nicotinic acid[J].Journal of Analytical Chemistry, 2019, 74:659-671.
[16] 严华, 崔凤云, 别玮, 等.超高效液相色谱-同位素稀释质谱法同时测定婴幼儿配方奶粉中10种水溶性维生素[J].食品安全质量检测学报, 2020, 11(17):5871-5878. YAN H, CUI F Y, BIE W, et al.Simultaneous determination of 10 kinds of water soluble vitamins in infant formula by ultra performance liquid chromatography-isotope dilution mass spectrometry[J].Journal of Food Safety & Quality, 2020, 11(17):5871-5878.(in Chinese)
[17] PORTER K, LODGE J K.Determination of selected water-soluble vitamins (thiamine, riboflavin, nicotinamide and pyridoxine) from a food matrix using hydrophilic interaction liquid chromatography coupled with mass spectroscopy[J].Journal of Chromatography B, 2021, 1171:122541.
[18] EL-HAWIET A, ELESSAWY F M, EL DEMELLAWY M, et al.Green fast and simple UPLC-ESI-MRM/MS method for determination of trace water-soluble vitamins in honey:greenness assessment using GAPI and analytical eco-scale[J].Microchemical Journal, 2022:107625.
[19] CHIRKIN V A, KARPOV S I, SELEMENEV V F.Effect of eluant composition on the retention of water-soluble vitamins in reversed-phase high-performance liquid chromatography[J].Journal of Analytical Chemistry, 2013, 68(4):341-347.  
[20] CHAMSEDDIN C, JIRA T.Evaluation of the chromatographic performance of conventional, polar-endcapped and calixarene-bonded stationary phases for the separation of water-soluble vitamins[J].Chromatographia, 2013, 76(9):449-457.
[21] PHINNEY K W, RIMMER C A, THOMAS J B, et al.Isotope dilution liquid chromatography-mass spectrometry methods for fat-and water-soluble vitamins in nutritional formulations[J].Analytical Chemistry, 2011, 83(1):92-98.  
[22] PHILLIPS M M.Liquid chromatography with isotope-dilution mass spectrometry for determination of water-soluble vitamins in foods[J].Analytical and Bioanalytical Chemistry, 2015, 407(11):2965-2974.  
[23] 中华人民共和国农业农村部.中华人民共和国农业部公告第2625号[EB/OL].(2018-01-20)[2022-05-12].http://www.moa.gov.cn/nybgb/2018/201801/201801/t20180129_6135954.htm. Ministry of Agriculture and Rural Affairs of the People's Republic of China.Announcement No.2625 of the Ministry of Agriculture of the People's Republic of China[EB/OL].(2018-01-20)[2022-05-12] http://www.moa.gov.cn/nybgb/2018/201801/201801/t20180129_6135954.htm.(in Chinese).
[24] 国家卫生和计划生育委员会, 国家食品药品监督管理总局.食品安全国家标准食品中烟酸和烟酰胺的测定:GB 5009.89-2016[S].北京:中国标准出版社, 2016. National Health and Family Planning Commission, State Food and Drug Administration.Determination of nicotinic acid and nicotinamide in food:GB 5009.89-2016[S].Beijing:Standards Press of China, 2016.(in Chinese)
文章导航

/