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
|
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-C_(18)(150 mm×4.6 mm, 5μm)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。
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-C_(18) 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.
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-C_(18) 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.
引文
[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] Ordoňez 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
[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] Ordoňez 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