Waters ;, ;100 ml,50 (FW135), ; : 5.0 g, (DS-8510 DTH), 100 ml, ; (AvantiJ-E), ; (RE-52AA),, 100 ml, ;Milli-Q, Millipore ; 1.4 :ACQUITY UPL

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2 0 1 3 2 Journal of Chinese Institute of Food Science and Technology Vol. 13 No. 2 Feb.

1 Journal of Chinese Institute of Food Science and Technology Vol. 13 No. 2 Feb ,2 1* ( 1 福建农林大学食品科学学院福州福建省产品质量检验研究院福州 ) 采用超高效液相色谱 (UPLC) 技术, 建立金柑中柠檬苦素和诺米林的快速同时检测技术样品经二氯甲烷超声波提取,ACQUITY UPLC TM BEH C 18 色谱柱 (2.1 mm 100 mm,1.7 μm) 分离, 以乙腈 - 水 (45 55) 为流动相, 梯度洗脱, 流速 0.3 ml/min, 柱温 35, 检测波长 215 nm 柠檬苦素和诺米林可在 3 min 内实现同时分离测定柠檬苦素和诺米林分别在 1~1780 μg/ml 和 1~1720 μg/ml 范围内线性关系良好 (R 2 = ), 方法检出限分别为 1.65 μg/g 和 1.28 μg/g, 加标回收率分别为 97.19%~100.06% 和 95.35%~99.83%, 相对标准偏差 (RSD) 均小于 5% 本法分析时间短, 灵敏度高, 操作方便, 结果准确, 适用于金柑中柠檬苦素和诺米林的同时测定超高效液相色谱 ; 柠檬苦素 ; 诺米林 ; 金柑 (2013) ,,,,,,, [1] 6 mg/l, (ultra performance liquid chromatography,u-, PLC) HPLC 6 mg/l, 20 [2] [11],, UPLC [3-4],,,,, 1, 1.1 HPLC [5-6] Davis [7] TLC [8] UV [9] RIA :,,45 [10] Davis ;UV, 40, ;TLC 1.2, ;RIA (Limonin) (Nomilin),, SIGMA ; ( ) ( HPLC ) ( ), :, g g, : ml 1.78 mg/ml 1.72 mg/ml : (2009N2002) 1.3 :,,1980,, : ACQUITY UPLC,

2 Waters ;, ;100 ml,50 (FW135), ; : 5.0 g, (DS-8510 DTH), 100 ml, ; (AvantiJ-E), ; (RE-52AA),, 100 ml, ;Milli-Q, Millipore ; 1.4 :ACQUITY UPLC TM BEH C 18 (2.1 mm 100 mm,1.7 μm), Waters ; : V V (45 55); :35 ; :0.3 ml/min; :2 μl; : :215 nm; 1.5 : 5.0 g,, μm, 2 2.1,, PDA 200~400 nm ( 1 ), 215 nm, 215 nm [12],, h, ,, 1 h, 1 2 Table 1 The efficiency of different solvents Table 2 The efficiency of different method on extracting on extracting limonin and nomilin limonin and nomilin 溶剂柠檬苦素 /mg g -1 诺米林 / mg g -1 二氯甲烷丙酮乙醇提取方法时间 /h 柠檬苦素 /mg g -1 诺米林 /mg g -1 水浴提取超声波提取

3 超高效液相色谱法快速并同时检测金柑中柠檬苦素和诺米林 ,,, 2.35, 30%~50%, min 2.97 min 2 3, 45% 2.4 3,, Table 3 The linear range and regression equation of 2μL, the calibration curve for limonin and nomilin (μg/ml),, 3,4 线性范围 / 相关回归方程 Y=3970X+2080,Y= μg ml -1 系数 3490X+4380, R ~1 780 μg/ml, 柠檬苦素 1~1 780 Y = 3970X ~1 720 μg/ml, 诺米林 1~1 720 Y = 3490X (IUPAC), S/N>3 [13], 3 (S/N=3,LOD),, 4 (LOD) 1.65 μg/g 1.28 μg/g 97.19%~100.06%, (RSD)0.74%~2.25% %~99.83%,, (RSD)0.80%~3.36%,

4 Table 4 4 Result of addition recovery experiment 样品含量 /mg 添加量 /mg 测定量 /mg 回收率 /% 标准偏差 *(RSD)/% 柠檬苦素诺米林 *: n=5 2.7 UPLC HPLC UPLC,,,, 4.3~,, μg/ml, 5 UPLC 5 Fig.5,, (mg/g DW) 1~1 780 μg/ml 1~ The contents of limonin and nomilin in different samples(mg/g DW) 样品名称柠檬苦素诺米林脐橙琯溪蜜柚柑橘尤溪金柑 μg/ml, (R 2 =0.9999) [15] HPLC 16 min, 16 ml( 1.0 ml/min) UPLC,3 min 1, 0.9 ml( 0.3 ml/min),,, HPLC,U- PLC 2) UPLC, 3, 1) [12] [14]

5 超高效液相色谱法快速并同时检测金柑中柠檬苦素和诺米林 181 [1] Hashinaga F, Ejima H, Nagahama H, et al. Limonoids in citrus fruit I Seasonal changes of limonoid components in pokan. Tankan, early stasuma mandarin and nastsudaidai fruits[j]. Bull Fac Agric Kagashima Uinv, 1977, 27: [2],,. [J]., 2005, (3): [3] Miller EG, Flanous R, Rivera-Hidalgo Fetal. The effect of citrus limonoids on hamster buccalpouch carcinogenesis [J]. Carcinogenesis, 1989, 10: [4] Miyake M, OzakiY, BennettR D, et al. Limonoid glucosides in calam on din seeds[j]. Phytochemistry, 1992, 31: [5] Negi P.S., Jayaprakasha G.K. Antibacteria activity of grapefruit Citrus paradisi peel extract[j]. Eur Food Res Technol, 2001, 213: [6] Maria H.Ribeiro, Dirce Silveira, Suzana Ferreira -Dais. Selective adsorption of limonin and naringin from orange juice to natural and synthetic adsorbents[j]. Eur Food Res Technol, 2002, 215(6): [7],. [J]., 2001,(2): 14. [8] Ohta H. Thin-layer and high-performance liquid chromatographic analyses of limonoids and limonoid glucosides in Citrus seeds[j]. Chromatogr, 1993, 639: [9],. [J]., 1999, 18(5): [10] C.A. Mclntosh. Quantification of limonin and limonoate a-ring monolactone during growth and development of citrus fruit and vegetative tissues by radioimmunoassay[j]. ACS Syrup Ser, 2000, 758: 73. [11],,,. [J]., 2008, 18(5): [12],,,. [J]., 2004, 4 (1): [13],,,. [J]., 2008, 42(7): [14],,,. [J]., 2009, 9(1): [15],,,. [J]., 2007, 33(4): Study on Rapid Simultaneous Determination of Limonin and Nomilin in Kumquat Using Ultra-Performance Liquid Chromatography Meng Peng 1,2 Zheng Baodong 1* ( 1 Food Science College of Fujian Agriculture and Forestry University, Fuzhou Fujian Inspection and Research Institute for Product Quality, Fuzhou ) Abstract A method for the rapid simultaneous determination of limonin and nomilin in Kumquat by ultra performance liquid chromatography (UPLC) was developed. The limonin and nomilin in the samples were first extracted with methylene chloride by sonication. The analyses were performed on UPLC with an ACQUITY UPLC TM BEH C 18 column(2.1 mm 100 mm,1.7 μm), using acetonitrile-water (45 55, V/V) as the mobile phase at a flow rate of 0.3 ml/min. The column temperature is measured 35, with a detection wavelength of 215 nm. The two compounds were effectively separated by gadient elution and detected by PDA in 3 minutes. The Calibration curve were good linear in the range of 1 ~ μg/ml for limonin and 1~1 720 μg/ml for nomilin, the correlation coefficient were both The limits of detection(lod) were 1.65 μg/g and 1.28 μg/g. The additon recoveries were 97.19%~100.06% and 95.35%~99.83%, respectively. The relative standard deviations were less than 5%. The result indicated that the method is rapid, sensitive, convenient, accurate and may be used for determination of limonin and nomilin in kumquat. Key wods ultra performance liquid chromatography(uplc); limonin; nomilin; kumquat

70 陈伟珠, 等 : 超高压液相色谱法测定鱼油中的和 DHP-EE % (RSD 1.05 %) respectively. The RSD of repetition was 1.54 %(n=6) for and 1.25 %(n=6) for. This method was

70 陈伟珠, 等 : 超高压液相色谱法测定鱼油中的和 DHP-EE % (RSD 1.05 %) respectively. The RSD of repetition was 1.54 %(n=6) for and 1.25 %(n=6) for. This method was DOI 10.3969/j.issn.1005-6521.2013.08.019 Food Research And Development 2013 3 34 6 69 1 2 1 1 * 1 1 1 1. 361005 2. 361005 : 采用超高压液相方法检测鱼油中的二十碳五烯酸乙酯 () 和二十二碳六烯酸乙酯 (), 采用 UPLC BEH C18(2.1 mm 50 mm,1.7 μm)