《新會陳皮產(chǎn)地鑒定方法 電感耦合等離子體質(zhì)譜法（征求意見稿）》

2T/GAIAxxx—xxxx新會陳皮產(chǎn)地鑒定方法電感耦合等離子體質(zhì)譜法本文件規(guī)定了新會陳皮產(chǎn)地鑒定的電感耦合等離子體質(zhì)譜法。本文件適用于新會陳皮產(chǎn)地的鑒定。2規(guī)范性引用文件下列文件中的內(nèi)容通過文中的規(guī)范性引用而構(gòu)成本文件必不可少的條款。其中，注日期的引用文件，僅該日期對應(yīng)的版本適用于本文件；不注日期的引用文件，其最新版本（包括所有的修改單）適用于本文件?！吨腥A人民共和國藥典》（2020年版）DB4407/T70地理標(biāo)志產(chǎn)品新會陳皮GB∕T39486-2020化學(xué)試劑電感耦合等離子體質(zhì)譜分析方法通則3術(shù)語和定義下列術(shù)語和定義適用于本文件。3.1陳皮Citrireticulataepericarpium本品為蕓香科植物橘CitrusreticulataBlanco及其栽培變種的干燥成熟果皮。釆摘成熟果實(shí)，剝?nèi)」?，曬干或低溫干燥?.2新會陳皮Xinhuicitrireticulataepericarpium新會陳皮為地理標(biāo)志產(chǎn)品保護(hù)范圍內(nèi)栽培的茶枝柑（Citrusreticulata‘Chachi’）的果皮經(jīng)曬干或烘干，并在保護(hù)區(qū)域范圍內(nèi)貯存陳化三年以上稱為新會陳皮。按采收加工時(shí)間可分為：柑青皮（青皮）、微紅皮（二紅皮）和大紅皮（紅皮）。新會陳皮的地理標(biāo)志產(chǎn)品保護(hù)范圍為廣東省江門市新會區(qū)會城街道辦、大澤鎮(zhèn)、司前鎮(zhèn)、羅坑鎮(zhèn)、雙水鎮(zhèn)、崖門鎮(zhèn)、沙堆鎮(zhèn)、古井鎮(zhèn)、三江鎮(zhèn)、睦洲鎮(zhèn)、大鰲鎮(zhèn)和江門市濱海新區(qū)管委會（原圍墾指揮部）現(xiàn)轄行政區(qū)域。4方法原理植物在生長過程中通過根系吸收土壤及水中的元素，元素組成與其生長地的地理特征密切相關(guān)，因此，依據(jù)陳皮中的礦物元素組成特征對產(chǎn)地進(jìn)行鑒定。陳皮樣品經(jīng)消解后，電感耦合等離子體質(zhì)譜測定礦物元素含量。利用SIMCA軟件建立基于新會陳皮與非新會陳皮元素含量的正交偏最小二乘法判別分析（OPLS-DA）模型。通過模型預(yù)測未知樣品的分組情況，確定其是否為新會陳皮。3T/GAIAxxx—xxxx5試劑和材料除另有說明外，所用試劑均為優(yōu)級純，超純水為二次蒸餾水。5.1濃硝酸：UP級。標(biāo)準(zhǔn)品溶液：Li、B、Na、Mg、Al、P、K、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Rb、Sr、Y、Mo、Sn、Sb、Cs、Ba、La、Ce、Pr、NPb、U、Rh和Re共41種濃度為1000μg/mL單元素標(biāo)準(zhǔn)溶液或混合標(biāo)準(zhǔn)溶液。5.2工作標(biāo)準(zhǔn)儲備溶液：采用逐級稀釋的方法，用2%HNO3將元素標(biāo)準(zhǔn)溶液配制成相應(yīng)工作標(biāo)準(zhǔn)曲線溶液。各工作標(biāo)準(zhǔn)曲線溶液濃度如下：5.2.1標(biāo)準(zhǔn)溶液S1（P）濃度為：0.0、0.1、0.5、1.0、5.0、10.0、20.0μg/mL；5.2.2標(biāo)準(zhǔn)溶液S2（Na、Ca、K、Mg）濃度為：0.0、0.1、0.5、1.0、5.0、10.0、20.0μg/mL；5.2.3標(biāo)準(zhǔn)溶液S3（Li、B、Al、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Rb、Sr、Sn、Sb、Cs、Ba、Tl、Pb、U）濃度為：0.0、0.1、0.5、1.0、5.0、10.0、50.0、100.0、200.0、500.0μg/L；1.0、5.0、10.0、50.0μg/L；5.2.5標(biāo)準(zhǔn)溶液S5（Mo）濃度為：0.0、0.5、1.0、2.0、5.0、10.0μg/L。5.3內(nèi)標(biāo)溶液采用逐級稀釋的方法，用2%HNO3將Rh和Re元素標(biāo)準(zhǔn)溶液配制成0.5μg/mL的混標(biāo)內(nèi)標(biāo)溶液。6儀器設(shè)備6.1電感耦合等離子體質(zhì)譜儀；6.2微波消解儀6.3分析天平：感量0.1mg。7測定步驟7.1礦物元素含量測定7.1.1樣品前處理取陳皮樣品，粉碎過二號篩，稱取約0.5g，精確至0.1mg，于聚四氟乙烯消解管中，加入5mL濃硝酸，放置30min后，放入微波消解儀中消解，于200℃消解25min，冷卻，取出消解管，于120℃趕酸約20min，消解液轉(zhuǎn)移到25mL比色管中，并用超純水定容到刻度。同時(shí)，按上述步驟進(jìn)行消解制備全流程空白。若元素濃度超出線性范圍則根據(jù)實(shí)際情況稀釋進(jìn)樣。7.1.2儀器參考條件7.1.2.1射頻功率：1550W；7.1.2.2采樣深度：8mm；4T/GAIAxxx—xxxx7.1.2.3霧化器：MicroMist；7.1.2.4霧化室溫度：2℃;7.1.2.5等離子體氣：15L/min；7.1.2.6輔助氣：0.8L/min；7.1.2.7載氣：1.03L/min；7.1.2.8碰撞氣：4.3mL/min；7.1.2.9蠕動泵轉(zhuǎn)速：0.1r/s；7.1.2.10測定礦物元素及質(zhì)量數(shù)：7Li、11B、23Na、24Mg、27Al、31P、39K、44Ca、47Ti、51V、52Cr、55Mn、56Fe、59Co、60Ni、63Cu、66Zn、75As、8141Pr、146Nd、147Sm、151Eu、157Gd、159Tb、163Dy、165Ho、166Er、172Yb、205Tl、208Pb、238U。7.1.3礦物元素標(biāo)準(zhǔn)曲線的繪制：在儀器最佳工作條件下，將上述配制的系列工作標(biāo)準(zhǔn)曲線溶液測定數(shù)據(jù)，以濃度為橫坐標(biāo)，待測元素響應(yīng)值（cps）與內(nèi)標(biāo)元素響應(yīng)值（cps）的比值為縱坐標(biāo)，繪制標(biāo)準(zhǔn)7.1.4礦物元素含量測定：在儀器最佳工作條件下，依次測定全流程空白和樣品溶液，以標(biāo)準(zhǔn)曲線法對樣品溶液中礦物元素進(jìn)行定量。陳皮中礦物元素含量按公式（1）計(jì)算。式中：Xk C樣品 C空白Vmk×（C樣品-C空白）×Vk×（C樣品-C空白）×V試樣中待測礦物元素含量，單位為毫克/千克（mg/kg）樣品溶液的稀釋倍數(shù)由回歸方程算得樣品溶液中礦物元素濃度，單位為毫克/升(μg/L）由回歸方程算得空白溶液中礦物元素濃度，單位為毫克/升(μg/L）樣品溶液定容體積，單位為毫升（mL）試樣的質(zhì)量，單位為克（g）7.2新會陳皮產(chǎn)地判別模型收集多批次新會陳皮與非新會陳皮，按照7.1中方法測定礦物元素含量。同時(shí)，若元素含量低于定量限（附錄A），則以定量限/2的數(shù)據(jù)計(jì)入結(jié)果。利用SIMCA軟件，建立正交偏最小二乘法判別分析(OPLS-DA）模型。元素含量以對數(shù)形式（Log10）轉(zhuǎn)換后計(jì)入模型。模型原始數(shù)據(jù)見附錄B。7.3陳皮產(chǎn)地鑒定7.3.1樣品礦物元素含量測定測定方法同上述7.1。5T/GAIAxxx—xxxx7.3.2產(chǎn)地判別將樣品元素含量導(dǎo)入7.2中的模型中，利用SIMCA的Predict功能進(jìn)行組別預(yù)測。以Preditionlist中的預(yù)測分組結(jié)果為準(zhǔn)。6T/GAIAxxx—xxxx附錄A附表1礦物元素定量限（ug/kg）15Ni52B5Nd3Na45556P57KY585955V55551555U157T/GAIAxxx—xxxx附錄B新會與非新會陳皮產(chǎn)地判別模型組元素含量（ug/kg）LiBNaMgAlPKCaTiVCrMnFeCoNiCuZnAsRbSrYXH-1166.752240826368960043023116800574182157635733504108932.92425111422922132.382549.659618.44861628.9761834560377.65XH-278.78210645625469036133891663472087241226971379180261.02510110363995825.19572.054659.27946421.6766284119644.73XH-3134.31257191223705158851587883920217385520805091859420.1524391103159732.50447.1212538.55743836.7051561857517.30XH-4292.452015844294651611826590563137140159765486662122833.70421129942861243.781811.933296.98837827.47946632059216.67XH-5258.0623469198392624975157706258461345815952014631076124112875823.731016.805497.011620915.691140924275103.31XH-691.62192573040145385631339386249931551918385714344446213.631204559010494142.71489.735765.89563963.8587082489362.78XH-7128.55209654309909556301444236575711401885580274236487264.611377867211494860.031123.9121432.22862258.8848183824786.36XH-8439.13172681972738038511691967311114893529429182770523.78483102732337047.751704.733269.01629017.92673717985XH-9674.71245251107196255082413162003717115165563734483024.68232114422441951.871323.549883.20668239.4587463296298.09XH-10168.01182104923779994191978969257914000176568969593229.27604185742953049.911349.2111770.56701918.8339463078772.51XH-1181.0527107455952139565172923635655127266557685046258260370036065935.83661.474710.041043728.9434423199347.02XH-12390.38228752095088118062824671098517694721383709884926.683171682632004242.543302.994437.13996425.442202222013116.09XH-13252.13166511380587653881758963731515413005438369938419.962392001325197151.052342.165051.38591717.651565533600XH-14242.99166826220678024493061566581313274101455835883942.00309164203588067.661019.4935795.38744220.0923522897693.02XH-15569.662692234675964241353459606399173935364327475195965.05349263194023086.991592.2920301.06746545.72636526046134.84XH-1673.65202396631569768002695073800914642287597145682842.263281009932836468.5611429.09426922.3147243688783.41XH-17841.15246281705558375692884995520042296355939845827994375.28145814377152902159.283309.175204.57901366.053919122698245.08XH-18279.0923609400344147380256796543983117515807582780175372.1757492264581044.22882.2913959.62498836.30526326694107.47XH-19234.583053256609158493224354645271138934824882649105527.12334210082561552.27971.255623.50809426.4231311717278.86XH-20116.27235354037949461761731497786314598639649118076523.35396108092347520.81727.682059.52449616.6931283307564.54XH-2170.88230421276319667223222277178616513830503654983346.1638075024425420.59313.595323.091021433.8996641954937.76XH-22694.17274152560017791751372078016420287824526671149319.0338285012741548.011410.547451.78866727.411942816225138.90XH-23156.04189631667637487391314262961515440674430454456613.4549692023610.75174.643080.34480010.58117581446012.20XH-2423.632627220564646075928355653882136231296357861123539.8365653266836717.77362.267328.80601557.3199161544237.82XH-2547.3328837819484826751980555475912004094549965685524.74382212042720329.77386.895311.18842527.8091674329948.06XH-2649.782262516100052489735199579887147520517103980146067.1436076484850526.55317.439352.13744345.74126082688444.19XH-27170.061703527755574968596537013551408770559271044588.9350351609017.60532.974485.16511826.4235753106720.11XH-28344.99199538976148963901733157360210773138582339271523.12139232392527.431002.1516740.30608521.7153846455175.34XH-29215071077216181301573059448113769742520522178316.39274107322241215.85303.072927.78646733.97152612316968.05XH-3087.9124407347527731541845183876211657038524920282122.35313114162509926.28453.2012584.79823328.4584963125573.40XH-31147.792674030099295887786667816931167886713888567138746.9844475275207251.94335.944856.12740655.102060211169479.478T/GAIAxxx—xxxxXH-32554.422332950371792699929965619557154753264832620117033.2853193283432037.041602.945049.37853446.071095732265153.25XH-33178.342818122780194083853860734616202694005816317235874.58546260314606456.601934.959140.42958739.401104748322144.66XH-341181.79215332180119606811155861985918805435445344849314.01244722029241.321550.314606.51922224.041067746242129.25XH-3590.07214645664407325731425047832114608768694039970918.35531175322269329.87466.082683.21675820.1052764993037.53XH-36102.89209331406385190233214345593516302471477213295834.88357104042846917.05356.922371.29608327.28114181266431.04XH-371404.812289579530138820917888850449176965133401202107623.97383122073038860.013169.4620719.939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