《新会陈皮产地鉴定方法 电感耦合等离子体质谱法（征求意见稿）》

2T/GAIAxxx—xxxx新会陈皮产地鉴定方法电感耦合等离子体质谱法本文件规定了新会陈皮产地鉴定的电感耦合等离子体质谱法。本文件适用于新会陈皮产地的鉴定。2规范性引用文件下列文件中的内容通过文中的规范性引用而构成本文件必不可少的条款。其中，注日期的引用文件，仅该日期对应的版本适用于本文件；不注日期的引用文件，其最新版本（包括所有的修改单）适用于本文件。《中华人民共和国药典》（2020年版）DB4407/T70地理标志产品新会陈皮GB∕T39486-2020化学试剂电感耦合等离子体质谱分析方法通则3术语和定义下列术语和定义适用于本文件。3.1陈皮Citrireticulataepericarpium本品为芸香科植物橘CitrusreticulataBlanco及其栽培变种的干燥成熟果皮。釆摘成熟果实，剥取果皮，晒干或低温干燥。3.2新会陈皮Xinhuicitrireticulataepericarpium新会陈皮为地理标志产品保护范围内栽培的茶枝柑（Citrusreticulata‘Chachi’）的果皮经晒干或烘干，并在保护区域范围内贮存陈化三年以上称为新会陈皮。按采收加工时间可分为：柑青皮（青皮）、微红皮（二红皮）和大红皮（红皮）。新会陈皮的地理标志产品保护范围为广东省江门市新会区会城街道办、大泽镇、司前镇、罗坑镇、双水镇、崖门镇、沙堆镇、古井镇、三江镇、睦洲镇、大鳌镇和江门市滨海新区管委会（原围垦指挥部）现辖行政区域。4方法原理植物在生长过程中通过根系吸收土壤及水中的元素，元素组成与其生长地的地理特征密切相关，因此，依据陈皮中的矿物元素组成特征对产地进行鉴定。陈皮样品经消解后，电感耦合等离子体质谱测定矿物元素含量。利用SIMCA软件建立基于新会陈皮与非新会陈皮元素含量的正交偏最小二乘法判别分析（OPLS-DA）模型。通过模型预测未知样品的分组情况，确定其是否为新会陈皮。3T/GAIAxxx—xxxx5试剂和材料除另有说明外，所用试剂均为优级纯，超纯水为二次蒸馏水。5.1浓硝酸：UP级。标准品溶液：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种浓度为1000μg/mL单元素标准溶液或混合标准溶液。5.2工作标准储备溶液：采用逐级稀释的方法，用2%HNO3将元素标准溶液配制成相应工作标准曲线溶液。各工作标准曲线溶液浓度如下：5.2.1标准溶液S1（P）浓度为：0.0、0.1、0.5、1.0、5.0、10.0、20.0μg/mL；5.2.2标准溶液S2（Na、Ca、K、Mg）浓度为：0.0、0.1、0.5、1.0、5.0、10.0、20.0μg/mL；5.2.3标准溶液S3（Li、B、Al、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Rb、Sr、Sn、Sb、Cs、Ba、Tl、Pb、U）浓度为：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标准溶液S5（Mo）浓度为：0.0、0.5、1.0、2.0、5.0、10.0μg/L。5.3内标溶液采用逐级稀释的方法，用2%HNO3将Rh和Re元素标准溶液配制成0.5μg/mL的混标内标溶液。6仪器设备6.1电感耦合等离子体质谱仪；6.2微波消解仪6.3分析天平：感量0.1mg。7测定步骤7.1矿物元素含量测定7.1.1样品前处理取陈皮样品，粉碎过二号筛，称取约0.5g，精确至0.1mg，于聚四氟乙烯消解管中，加入5mL浓硝酸，放置30min后，放入微波消解仪中消解，于200℃消解25min，冷却，取出消解管，于120℃赶酸约20min，消解液转移到25mL比色管中，并用超纯水定容到刻度。同时，按上述步骤进行消解制备全流程空白。若元素浓度超出线性范围则根据实际情况稀释进样。7.1.2仪器参考条件7.1.2.1射频功率：1550W；7.1.2.2采样深度：8mm；4T/GAIAxxx—xxxx7.1.2.3雾化器：MicroMist；7.1.2.4雾化室温度：2℃;7.1.2.5等离子体气：15L/min；7.1.2.6辅助气：0.8L/min；7.1.2.7载气：1.03L/min；7.1.2.8碰撞气：4.3mL/min；7.1.2.9蠕动泵转速：0.1r/s；7.1.2.10测定矿物元素及质量数：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矿物元素标准曲线的绘制：在仪器最佳工作条件下，将上述配制的系列工作标准曲线溶液测定数据，以浓度为横坐标，待测元素响应值（cps）与内标元素响应值（cps）的比值为纵坐标，绘制标准7.1.4矿物元素含量测定：在仪器最佳工作条件下，依次测定全流程空白和样品溶液，以标准曲线法对样品溶液中矿物元素进行定量。陈皮中矿物元素含量按公式（1）计算。式中：Xk C样品 C空白Vmk×（C样品-C空白）×Vk×（C样品-C空白）×V试样中待测矿物元素含量，单位为毫克/千克（mg/kg）样品溶液的稀释倍数由回归方程算得样品溶液中矿物元素浓度，单位为毫克/升(μg/L）由回归方程算得空白溶液中矿物元素浓度，单位为毫克/升(μg/L）样品溶液定容体积，单位为毫升（mL）试样的质量，单位为克（g）7.2新会陈皮产地判别模型收集多批次新会陈皮与非新会陈皮，按照7.1中方法测定矿物元素含量。同时，若元素含量低于定量限（附录A），则以定量限/2的数据计入结果。利用SIMCA软件，建立正交偏最小二乘法判别分析(OPLS-DA）模型。元素含量以对数形式（Log10）转换后计入模型。模型原始数据见附录B。7.3陈皮产地鉴定7.3.1样品矿物元素含量测定测定方法同上述7.1。5T/GAIAxxx—xxxx7.3.2产地判别将样品元素含量导入7.2中的模型中，利用SIMCA的Predict功能进行组别预测。以Preditionlist中的预测分组结果为准。6T/GAIAxxx—xxxx附录A附表1矿物元素定量限（ug/kg）15Ni52B5Nd3Na45556P57KY585955V55551555U157T/GAIAxxx—xxxx附录B新会与非新会陈皮产地判别模型组元素含量（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-371404.812289579530138820917888850449176965133401202107623.97383122073038860.013169.4620719.93917219.365282329433146.41XH-38452.16336696288495844741433562990012731071858033455225.931159132183245831.42584.29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