]2‡…3—– · stuvw,;xyz{|,}~ •†\]2‡…3—– › fi,fl°(,– †,–...

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stuvw,;xyz{|,}~\]23 ¯°(±² ±³´µ#¶·¸¹º±»¼ é5#$%&'(+,12#3é5é. 550009 67 ./½¾¿ÀÁ=ÂÃÄÅ]=ÆBC/Ç%ÈÉZ[CÊË。[ FGÌÍÇ%ÈÎÏGÐÑÒ45Á=MNÓ 284 LÔRÕÖu×ØGPLS ½Ê[CÙÚÛÜ2K/¿ÀÁ=/ÂÃÄÅÝÞÅ]=ÆBCß[ÎÏK;O 9002.45~4069.19cm -1 QRàáâã^y Savitzky-Goly SG äåæçèÎÏéêzëìíÊËîïðñòóôFG]Ç% ÈFGZõ/^_çèí<ö。[ ^_¿ÀÁ=/hÅÝÞÅ÷øéZÊË/ùúûã üO 0.9968 0.9872 0995 ýþÿ!"F#RMSECV üO 0.354 0.558 0.067 。[ ^vÊËîïð$%÷FG&'()*#+Ç%ÈFG,y=~ /ÂÃÄÅ]=Æ-É[C89: =~ÂÃÄÅÇ%È[CÊË ;<=>? TS41 1  @ABCD A  @EF? 0517-6611 2017 15-0079-04 EstablishmentofNearinfraredQuantitativeModelforQuickTestofWatersolubleSugarandNicotineinFluecuredTobaccoin Guizhou DUANKai JIHouwei LIUJian etal TechnologyCenterofChinaTobaccoGuizhouIndustrialCo.Ltd Guiyang Guizhou550009 Abstract Objective Toestablishnearinfraredquantitativemodelfordetectionofwatersolublesugarandnicotineinfluecuredtobacco. Method Basedonnearinfraredspectroscopy atotalof284sampleswereselected andpartialleastsquares PLS modelwasusedtoes tablishmodel solublesugar totalsugar reducingsugar andnicotinecontentintobaccoinGuizhouwerequantitativelyanalyzed thespectral rangewasdeterminedas9002.45-4069.19cm -1 spectralpretreatmentwasconductedbyusingfirstorderderivativeandSavitzky-Goly SG smoothingfilter.Theprecisionofthemodelwasinvestigated theresultsobtainedbystandardmethodandnearinfraredmethodwere compared. Result Thecorrelationcoefficientsoftotalsugar reducingsugarandnicotineintobaccowere0.9968 0.9872 0.9951 RM SECVwere0.354 0.558 0.067respectively. Conclusion Theprecisionofthemodelisgood andthereisnosignificantdifferencebe tweenthetwomethods.Thenearinfraredmethodissuitablefortherapidquantitativeanalysisofwatersolublesugarandnicotineintobacco. Keywords Tobacco Watersolublesugar Nicotine Nearinfrared Quantitativemodel KLMN 1986 —), .ÙÚÙ/0z,=~9 01 ¡¢£c5,=~= 1901OPQR 2017-03-13 êë¼12NIR í®Vìí12W'î ïð§ñò§ói?ôõìkÍ¢höj ÷ÏêÖlyøùMúû4üªñËý&þ:¾0ÿ oh !" ÎÇùðFñ^D# ` h1nêë¼ÀÚV¤ÏÓø' P^DVêë¼#$nsʤު«¢q¢¯Í¢ V12wxÒ% &6 780~2500nmá¢'ïêë ¼á ${©ï¡()q¸VýoÎjk:9Uì# ®'8¯VCH 、—OH 、—NHh*1 ${#°ù±l+$,-.hjk:9UìF/0$©D¯ V1Pk122'Îwxn${V%ý3&W' P8Vðö£45' 67:9Uì#V°ù ±l+$,m®'8¯V® 1²-.h§P8< hÎÌ'P1L]VT9ßzj8¯V:9#$ Î#¶}q±°ù±V®¯F:¢$_ØVj k³El^,$,®¯F:¢$_;<=Vjk ³E½$,®¯<=þ;ã>®¯? @q8$ABh ³ÈÉ/$C&oÿ Qý$$#¶}q±$,Dïjkbc2'EßnU o/$D¯VF¾W'sGPkV5'ÈÉ«&n PkV:9Uìjk°FHIJÑVKLìíª« MÍÎåNOPQR6)*ST¯8ð·²Ã n<=¨Uñò 7-9 ²êë¼12ìí³Î>UN?kMÍô í®<ØV÷ÏêVÖl|${:9Uììí`D ¯F¾hô!è`¦WVªñXYZh 10 ñêë¼ 12[Í/$jK$_Vab$,\]^h 11 ñ _`©êë¼6ì9FT-NIR îMÍ¢$©`$a#V by,tch 12 Ëêë¼dø[Í${eN®¯¡ë &h 13-14 ñêë¼ìí12|fgÍ$aVD¯2 'Ë|fêë¼ìí12n 67$a:9Uì ª«£MÍÞßËêë¼12hI 2015 Öé 5ijk$©ÒV 284 êQý$$ëoL]jyþEk  PLS lmn¶}q±$,®¯ª«¢¯ìínñ£ 4ëonmûVѪqª«Üoî|ï#©QýC&nQ ý$$D¯VF¾ôõ12pq1 STUVW 1.1 ST 1.1.1 jk9:rsAntaris _`©«têë¼6ì9 Thermo ½/), ÿ'ìuHë`ëovwHëÐÑTQAnalyst7.0 :9@¯9xRFutura p8LKLìí9 Allliance  / ); FED -240û IJ; } FETUL Binder y/); YC-400B-03 ûz{9M${NOP |¤}U~); AE100 û;<ìí=ãMettler-Toledo } ); 40 È'^1.1.2 ëofÒQý0ÚÌ 2015 Öé5ijk$© ÒVQý$$ëo 284 êëoWé5iVjk $©ÒjkhÓëo#$Û¶ abcdefJournalofAnhuiAgri.Sci.2017 45 15 ): 79-82 87

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Page 1: ]2‡…3—– · stuvw,;xyz{|,}~ •†\]2‡…3—– › fi,fl°(,– †,– ‡,·µ#,¶ •,‚„”,–»… (Ø5#$%&’(+,12#3,Ø5Ø. 550009) 67

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 TS41+1  @ABCD

 A  @EF?

 0517-6611(2017)15-0079-04

EstablishmentofNearinfraredQuantitativeModelforQuickTestofWatersolubleSugarandNicotineinFluecuredTobaccoinGuizhouDUANKai,JIHouwei,LIUJian etal (TechnologyCenterofChinaTobaccoGuizhouIndustrialCo.Ltd,Guiyang,Guizhou550009)Abstract [Objective]Toestablishnearinfraredquantitativemodelfordetectionofwatersolublesugarandnicotineinfluecuredtobacco.[Method]Basedonnearinfraredspectroscopy,atotalof284sampleswereselected,andpartialleastsquares(PLS)modelwasusedtoestablishmodel,solublesugar(totalsugar,reducingsugar)andnicotinecontentintobaccoinGuizhouwerequantitativelyanalyzed,thespectralrangewasdeterminedas9002.45-4069.19cm-1,spectralpretreatmentwasconductedbyusingfirstorderderivativeandSavitzky-Goly(SG)smoothingfilter.Theprecisionofthemodelwasinvestigated,theresultsobtainedbystandardmethodandnearinfraredmethodwerecompared.[Result]Thecorrelationcoefficientsoftotalsugar,reducingsugarandnicotineintobaccowere0.9968,0.9872,0.9951,RMSECVwere0.354,0.558,0.067respectively.[Conclusion]Theprecisionofthemodelisgood,andthereisnosignificantdifferencebetweenthetwomethods.Thenearinfraredmethodissuitablefortherapidquantitativeanalysisofwatersolublesugarandnicotineintobacco.Keywords Tobacco;Watersolublesugar;Nicotine;Nearinfrared;Quantitativemodel

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,JournalofAnhuiAgri.Sci.2017,45(15):79-82,87    

Page 2: ]2‡…3—– · stuvw,;xyz{|,}~ •†\]2‡…3—– › fi,fl°(,– †,– ‡,·µ#,¶ •,‚„”,–»… (Ø5#$%&’(+,12#3,Ø5Ø. 550009) 67

g

1 XY��

Table1 Informationofsamples

�Ò

Producingareaêd

Number∥ê

hÓêd

Gradenumber

�-��

Zheng’anWuchuan 10 3����

ShibingZhenyuan 7 4��

Bijie 5 1��

Weining 37 4-�

Anshun 23 4�~

Kaidu 28 5�¶

Huishui 8 8�"

Qiannan 16 5��

Xingpan 30 5�'

Zunyi 15 3=�

Tianzhu 15 4��¶

Liupanshui 6 2��

Panxian 20 7��"

Qianxinan 49 5�5"

Qiandongnan 15 5ëold

Totalsample 284 —

  _'ëom%&${«&'�

YC/T31—1996[15] $

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 %&${«&'�

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Table2 StatisticsofmainchemicalconstituentsintobaccoinGuizhou

bycontinuousflowmethod %

:9Uì

Chemicalconstituenty8w

Maximumyþw

Minimummw

Mean'�jt

Standarddeviation

Totalsugar 35.11 13.14 24.52 4.49

°ù±

Reducingsugar 29.78 11.14 21.14 3.73

l�^,

Nicotine 3.27 1.43 2.21 0.33

1.3 ~������

 ïØoy8(�Ò�þ6ìHÌ�

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《GB/T29858—2013ì<6ìôO¢�

¢¯ìíà�

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10000~4000cm-1(1000~2500nm);

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Fig.1 Samplespectrum

ì_´®V'ð¤Þ#$

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Table3 Effectofdifferentspectralpretreatmentsonpredictionresults

oftotalsugarmodel

[¸ð! 

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(r)Correlationcoefficient

�Ô©ªÜo

m!t

Internalcrossvalidationvariance(RMSECV)

¡¹´d

Firstorderderivative 0.9965 0.370

¡¹´d

+Norrśdº&

FirstorderderivativeandNorrisderivativefilter

0.9908 0.601

¡¹´d

+SG㻺&

FirstorderderivativeandSavitzkyGolyfilter

0.9968 0.354

E¹´d

Secondorderderivative 0.9903 0.616

E¹´d

+Norriśdº&

SecondorderderivativeandNorrisderivativefilter

0.9921 0.557

E¹´d

+SG㻺&

SecondorderderivativeandSavitzkyGolyfilter

0.9872 0.708

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Page 3: ]2‡…3—– · stuvw,;xyz{|,}~ •†\]2‡…3—– › fi,fl°(,– †,– ‡,·µ#,¶ •,‚„”,–»… (Ø5#$%&’(+,12#3,Ø5Ø. 550009) 67

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Table4 Effectofdifferentwavelengthrangesontotalsugarpredic

tionmodel

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Spectralrange∥cm-1sÊÐd

(r)Correlationcoefficient

�Ô©ªÜo

m!t

Internalcrossvalidationvariance(RMSECV)

xR8L÷:hÅìá

Softwareautomaticoptimizationselection

0.9682 1.110

(4329.79~4350.62�

6140.24~5912.68)Ò%÷:hÅìá

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0.9968 0.354

(9002.45~4069.19)

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 Hñ�Ô©àÜo

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8cm-1。Hñ¡¹´dL]

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 n6쪫[¸ð

。l±

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ûsÊVdø2'½¶

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V

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,l±

、°ù±

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Table5 Relevantmathematicalindexofnearinfraredcalibrationmodel

:9Uì

Chemicalconstituents¢�ëǯ

Correctedsamplesize

y÷jUìd

Optimalprincipalcomponent

sÊÐd

(r)Correlationcoefficient

�Ô©ªÜom!t

Internalcrossvalidationvariance

[ÍCD

Predictionrange%

Totalsugar 277 9 0.9968 0.354 13.14~35.11°ù±

Reducingsugar 279 10 0.9872 0.588 11.14~29.78$,

Nicotine 272 11 0.9951 0.067 1.43~3.27

<

3 ¡{(f�U���\�®¯<

Table3 Scatterplotoftotalsugarchemicalvalueandmodel

predictivevalue

2.5 ��°±²³´

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3ê

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,ìÝêÄ

1#、2#、3#, êëoAB

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6_�

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(RSD)mþË

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Table4 Scatterplotofreducingsugarchemicalvalueandmodel

predictivevalue

2.6 B·VWU~��VW+¸

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Page 4: ]2‡…3—– · stuvw,;xyz{|,}~ •†\]2‡…3—– › fi,fl°(,– †,– ‡,·µ#,¶ •,‚„”,–»… (Ø5#$%&’(+,12#3,Ø5Ø. 550009) 67

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Table5 Scatterplotofnicotinestandardvalueandcalculated

value

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Table6 PrecisionexperimentsresultofNIRcorrectionmodels %

ëo

Sample:9Uì

Chemicalconstituent

AB|d

Scanningtimes

1 2 3 4 5 6 7 8 9 10mw

Meansn'�jt

Relativestandarddeviation(RSD)

1#l±

  27.62 27.59 27.58 27.60 27.61 27.59 27.58 27.62 27.59 27.61 27.59 1.45°ù±

17.24 17.20 17.23 17.20 17.20 17.21 17.24 17.22 17.19 17.21 17.21 1.69$,

  2.17 2.16 2.19 2.20 2.18 2.17 2.19 2.16 2.20 2.19 2.18 1.452#

  32.33 32.34 32.33 32.30 32.32 32.30 32.31 32.31 32.33 32.34 32.32 1.45°ù±

23.09 23.07 23.06 23.07 23.06 23.08 23.07 23.09 23.08 23.07 23.07 1.02$,

  2.26 2.27 2.26 2.24 2.25 2.26 2.25 2.23 2.23 2.27 2.25 1.403#

  18.95 18.96 18.97 18.98 18.95 18.96 18.96 18.95 18.96 18.97 18.96 0.95°ù±

12.15 12.16 12.15 12.17 12.18 12.19 12.16 12.16 12.15 12.18 12.16 1.36$,

  1.83 1.82 1.80 1.83 1.82 1.81 1.81 1.83 1.82 1.85 1.82 1.33

g

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Table7 Resultsofsolublesugarandnicotineby2methods %

ëoêÄ

SampleNo.

Totalsugar'�! 

Standardmethod

êë¼6ì 

NIRsnjt

Relativedeviation

°ù±

Reducingsugar'�! 

Standardmethod

êë¼6ì 

NIRsnjt

Relativedeviation

$,

Nicotine'�! 

Standardmethod

êë¼6ì 

NIRsnjt

Relativedeviation

1 28.27 28.22 3.54 24.21 24.19 1.41 2.35 2.33 1.412 25.90 25.83 4.95 20.69 20.71 1.41 1.78 1.82 2.833 25.73 25.69 2.83 20.63 20.66 2.12 1.74 1.80 4.244 26.33 26.35 1.41 20.90 20.93 2.12 1.73 1.71 1.415 24.66 24.70 2.83 19.92 20.01 6.36 1.57 1.61 2.836 25.89 25.91 1.41 21.02 20.98 2.83 2.13 2.09 2.837 23.23 23.16 4.95 18.99 19.03 2.83 2.04 2.06 1.418 24.81 24.77 2.83 20.16 20.14 1.41 2.08 2.05 2.129 24.89 25.01 8.49 19.45 19.45 0.00 2.05 2.03 1.4110 22.73 22.68 3.54 18.50 18.46 2.83 2.09 2.06 2.1211 18.40 18.33 4.95 15.71 15.68 2.12 1.77 1.81 2.8312 20.67 20.62 3.54 17.81 17.82 0.71 1.75 1.76 0.7113 21.35 21.33 1.41 19.33 19.32 0.71 3.12 3.13 0.7114 22.53 22.58 3.54 20.48 20.52 2.83 3.08 3.10 1.4115 21.66 21.63 2.12 20.07 20.05 1.41 2.99 3.03 2.8316 29.33 29.34 0.71 25.62 25.59 2.12 2.28 2.31 2.1217 27.66 27.62 2.83 23.94 24.00 4.24 2.26 2.24 1.4118 27.46 27.45 0.71 23.45 23.41 2.83 2.41 2.39 1.4119 28.47 28.51 2.83 24.71 24.71 0.00 2.35 2.33 1.4120 29.97 30.02 3.54 26.20 26.23 2.12 2.21 2.19 1.41

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��

Concentrationmg/L

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Absorbancevalue

��

Concentrationmg/L

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Absorbancevalue

0 1187 1.2 1204990.4 44781 1.6 1568050.8 82512 2.0 192283

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