206 5 (5μm,4.6mm 50 mm),, 276nm, 20 μl,, 30,, 0.8mL/min, ( 2080,585,090) (patulin) (2) : AltimaTM C8 (5μm, 4.6mm 50mm),, 276nm, 20μL 30, [2], 090, (.0
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1 Vol.32,No.5 May2 0 6 DOI:0.3652/j.issn HPLC OptimizationonHPLCdetectionandpre-treatment conditionsofpatulininfreshapple SUN Li-hua CHEN Ji-luan 2,3 QIAN Hui-ping LI Zhi-wen 2,3 4 2,3 PANG Xue-qun 4 YAN Shi-jie 2,3 (., , , ) (.Food ColegeShihezi University,Shihezi,Xinjiang832003,China 2.Colegeof Food Scienceand BiologicalEngineering,Tianjin Agricultural University,Tianjin300384,China 3.Tianjin Engineering and Technology Research Centerof AgriculturalProducts Procesing,Tianjin300384,China 4.Colegeof Biotechnology,South China Agricultural University,Guangzhou,Guangdong50642,China) : rateforhplc whichalwaysafectthesensitivityandanalysisefi-, HPLC ciencyofthemethodwereoptimizedsystemicaly.theresultsindica- tedthatsolidphaseextraction(spe)techniquesusingfunctionalized : polystyrene-divinylbenzenecolumn (PEP)exhibitedsatisfactoryre- coveriescomparingwithotherextraction methods.undertheopti- =0 90, 0.8 ml/min HPLC, mizedchromatographicconditions,patulincouldbe welseparated fromotherimpuritieswithin4 min,anddetectedwithawidelinear, (8.9%), rangebetween μg/landadetectionlimitof0μg/l (S/ PEP-SPE N=3)usingacetonitrile/water(90:0,v/v)asmobilephase,0.8 (82.42%~95.57%) (3.26% ~4.4%), ml/minasflowrate.theproposedpep-spe-hplc methodwas, PEP-SPE furtherappliedtothedeterminationofpatulininfreshapplesinthe HPLC rangeof82.42%-95.57%,indicatingitmightserveasaneficient toolfortheaccuratequantificationofpatulininfoodsamples. Keywords:high performanceliquid chromatographysolid-phase : Abstract:Arapidandsensitivemethodwasestablishedfortheaccu- ratedeterminationofpatulininfreshapples.experimentalparame- tersincludingextractionmethods,mobilephasecompositionandflow, : ( :205BAD6B07) ( : 5JCYBJC5300),, :,, : (97-),,, yanshijie@26.com : patulinfreshapple [], 53
2 206 5 (5μm,4.6mm 50 mm),, 276nm, 20 μl,, 30,, 0.8mL/min, ( 2080,585,090) (patulin) (2) : AltimaTM C8 (5μm, 4.6mm 50mm),, 276nm, 20μL 30, [2], 090, (.0,0.8, 0.6mL/min) [3], mg 50μg/kg [4] [9], 50000μg/L SN/T , 0,50,, 00,250,500,000,5000,0000,25000μg/L, 0 [5-6],.2.3,, 0.0g, ml000μg/l (SPE HPLC) A [7] ( A 25 ml, 25 Mycrosep 228AflaPat 40kHz 300 W 30 min) 78%~7%,RSD 2.~8.2%, ( A 3 ml, 2h, 2mL,, 25 ml, ) ( Wu [8] A 25mL,, ) ( (), 80.7% ~ 25 ml,, ), 8.45%, 8000r/min 5min, HPLC [0], HPLC.2.4,, PEP () (LLE): [0], : ml,.. 5mL 0mL, min :85( 85 mm),, ( 0 ml),, 3 : 98%, TRC, 5 ml : 2600PG/mL, 5mL, :, Fisher, 5g :,, 5 ml , 40 :LC-200,,mL,0.45μm :RE-2000 ml HPLC :Visiprep TM SPE-2, Supelco (2)PEP (PEP-SPE): 2 ml :KQ-500DE,2mL,, mL, :NY3022L, Origin Membranes , 00 ml [] ml ml [2] ml, ml () : AltimaTM C8 ml,
3 32 5 : HPLC,, ml 090,0.45μm ml 2..2, HPLC.2.5,,, 0.0g, 50,00,000μg/L3, 0.8 ml/min, ml, min 3, ~25000μg/L ( 3) 2 2 :, 2. Y = X +4.49, R = (n=9) 000μg/L,, 6, 0.53RSD 0.072%, [3] : 3, 0μg/L [4] Agilent00ODS 20% 0% 3.850~6.372 min, (5μm,50mm 4.6mm ), , ml/min,zaied 80,585 [5] SpherisorbODI, 090, ml/min Figure Efectofdiferentmobilephase 2 ratioonseparation Figure2 Efectofdiferentflowratioonseparation 55
4 Figure3 Standardcurveofpatulin : 8.90% 65.38% (P>0.05), (P<0.05), [6], 5 HPLC 65.37% OH H, Figure5 Efect of diferent purification techniques on, VA HPLCseparationforpatulininfreshapple VC, [7]2-22 [8] [7]23-24 :LLE PEP-SPE PEP-,, SPE 82.42%~95.57%,,,, LLE 78.54% ~80.73%,PEP-SPE 3 (P<0.05) 2.3 LLE PEP-SPE LLE, 2.3. HPLC 5 :PEP-SPEC :PEP-SPE LLE,,,PEP-SPE 6.372min LLE min /7, [9], 96mL, 56 PEP 82.42% ~95.57%,,Beltran [20] LLE 7%~75%,Gaspar [2] LLE PEP-SPE Table LLEandPEP-SPErecoveriesandcoeficient ofvariation / LLE PEP-SPE ( μ g L - ) /% /% /% /% a b a b 3.26 Figure4 Efectofdiferentextractionmethodson a b 4.4 recoveries
5 32 5 : HPLC 60% PEP-SPE[7],,,. PEP-SPE,, [J].,2009,25():27-3., [8]WuRi-na,HanFeng-lan,ShangJie,etal.Analysisofpatulin PEP- SPE 5min, 60 inappleproductsbyliquid-liquidextractionsolidphaseextrac- tionand matrixsolid-phasedispersion methods:acomparative 2, study[j].eur.foodres.technol.,2009(228): PEP-SPE,PEP-SPE [9]GokmenV,AcarJ,SariogluK.Liquidchromatographicmethod forthedeterminationofpatulininapplejuiceusingsolid-phase Boonzaaijer [22] C8 extraction[j].analyticachimicaacta.,2005,543:64-69., 63%,RSD [0]Cho M S,Kim K,SeoE,etal.Occurrenceofpatulininvari- 7%26 ml PEP-SPE 82.42~95.57%,RSD 3.26~4.4%, ousfruitjuicesfromsouthkorea:anexposureassessment[j]. FoodSci.Biotechnol.,200,9():-5. 8 ml PEP-SPE [],,,. SPE HPLC Boonzaaijer [22], C8 [J].,2007(5): [2]LiJian-ke,WuRi-na,Hu Qiu-hui,etal.Solid-phaseextrac- tionandhplcdeterminationofpatulininapplejuiceconcen- 2 LLE PEP-SPE trate[j].foodcontrol,2007,8: Table2 Comprehensive comparison with PEP-SPE and LLEpurificationtechniques [3]LiTP,SakaiR,ManafN A,etal.Highperformanceliquid chromatography methodforthedeterminationofpatulinand / 5-hydroxymethylfurfuralinfruitjuices marketedin Malaysia /ml % /% /min [J].FoodControl,204,38: LLE ~ ~ [4],,. PEP-SPE ~ ~4.4 5 [J].,2007,23(5): [5]ZaiedC,AbidS,HlelW.Occurrenceofpatulininapple-based- 3 foodslargelyconsumedin Tunisia[J].Food Control,203, 3: , HPLC [6]. : ml/min [D]. :,200:38-4. PEP [7]. [D]. : 82.42%~95.57%, % ~4.4%, [8],,,. [J].,2009,40(9): [9],,,., [J].,2008,5(3):50-5. [20]BeltranE,IbanezM,SanchoJV,etal.Determinationofpatu- []. [D]. : [J].FoodChemistry,204,42: ,204:5-6. [2]GasparE M S M,LucenaA FF.ImprovedHPLC methodology [2],. [J].,989,8 forfoodcontrol-furfuralsandpatulinasmarkersofquality[j]. (2): FoodChemistry,2009,4: [3]. [22]BoonzaaijerG,BobeldijkI,Osenbruggen W A.Analysisof [D]. :,2008:-2. [4]AbdorrezaM,RouyaT,MarziehK,etal.Enzyme-assistedex- tractionandionicliquid-baseddispersiveliquid-liquid microex- tractionfolowedbyhigh-performanceliquidchromatographyfor determinationofpatulininapplejuiceand methodoptimization usingcentralcompositedesign[j].analytica Chimica Acta., 203,804:04-0. [5],,. [J].,2007,7(/2): [6],. [J].,2003,3():8-9. lininappleandderivedproductsby UHPLC MS/MS:study ofmatrixefectswithatmosphericpressureionisationsources patulinindutchfood,anevaluationofaspe based method [J].FoodControl,2005,6:
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SUPPORTING INFORMATION Trichodermides A E: New Peptaibols isolated from Australian Termite Nestderived Fungus Trichoderma virens CMB-TN16 Wei-Hua Jiao,, Zeinab Khalil, Pradeep Dewapriya, Angela A. Salim,
Supporting information. An unusual bifunctional Tb-MOF for highly sensing of Ba 2+ ions and remarkable selectivities of CO 2 /N 2 and CO 2 /CH 4
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Study on Purification Technology and Antioxidant Activity of Total Flavonoid from Eriobotryae Folium
Interleukin-1beta causes pulmonary inflammation, emphysema, and airway remodeling in the adult murine lung [J]. Am J Respir Cell Mol Biol, 2005, 32(4): 311-318. [10] FAN C H, LI S Y, LI M, et al. The clinical
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FENXI HUAXUE Chinese Journal of Analytical Chemistry. Savitzky-Golay. n = SG SG. Savitzky-Golay mmol /L 5700.
38 2010 3 FENXI HUAXUE Chinese Journal of Analytical Chemistry 3 342 ~ 346 DOI 10. 3724 /SP. J. 1096. 2010. 00342 Savitzky-Golay 1 * 1 2 1 3 1 1 510632 2 510632 3 200444 PLS Savitzky-Golay SG 10000 ~ 5300
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Preparation and Application of Amorphous Alloy Catalyst
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The straight-line navigation control of an agricultural tractor subject to input saturation
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Supporting Information
Supporting Information Synthesis and Electroactive Properties of Poly(amidoamine) Dendrimers with an Aniline Pentamer Shell Wei-I Hung a, Chih-Bing Hung a, Ya-Han Chang a, Jiun-Kuang Dai a, Yan Li b, Hai
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41 Vol.41, No. 01 RARE METAL MATERIALS AND ENGINEERING March 01 Pb O 4 PbO ( 710049) SnO -Sb Pb O 4 Pb O 4 100.5 h 970 h XRF XRD SEM Pb O 4 PbO PbO TG146.1 + A 100-185X(01)0-046-05 [1,] 1 PbO PbO Sn-Sb
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2010 37 6971 976 Acta Horticulturae Sinica 5 1,2 1,* 1 1 150040 2 150025 GC MS 23 30 11 64.73% α 30.67% 14.92% 13 61.41%α 28.98% 14.70%α 3 50 µl ml -1 5 100% µl ml -1 92% 85% 23% 5 µl ml -1 60% 25% 74%
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Electronic Supplementary Information DFT Characterization on the Mechanism of Water Splitting Catalyzed by Single-Ru-substituted Polyoxometalates
Electronic Supplementary Information DFT Characterization on the Mechanism of Water Splitting Catalyzed by Single-Ru-substituted Polyoxometalates Zhong-Ling Lang, Guo-Chun Yang, Na-Na Ma, Shi-Zheng Wen,
HS - SPME - GC - MS. Abstract: Objective A rapid method was developed for multi2residues determination of organochlorine and pyrethroids
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Fingerprint analysis of organic acids chromones and triterpenoid saponins in five Cimicifuga species by thin layer chromatography
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Supplementary information:
Supplementary information: Monitoring changes of docosahexaenoic acid-containing lipids during the recovery process of traumatic brain injury in rat using mass spectrometry imaging Shuai Guo 1, Dan Zhou
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