附件2 《含氨基酸水溶肥料 游離氨基酸含量的測(cè)定-分光光度法》（編輯說(shuō)明）

團(tuán)體標(biāo)準(zhǔn)含氨基酸水溶肥料游離氨基酸含量的測(cè)定—分光光度法編制說(shuō)明2022年10月15日?qǐng)F(tuán)體標(biāo)準(zhǔn)《含氨基酸水溶肥料游離氨基酸含量的測(cè)定—分光光度法》編制說(shuō)明1.工作簡(jiǎn)況1.1任務(wù)來(lái)源根據(jù)《廣西肥料協(xié)會(huì)關(guān)于下達(dá)2022年第二批團(tuán)體標(biāo)準(zhǔn)項(xiàng)目計(jì)劃的通知》（廣肥協(xié)[2022]5號(hào)）的要求，團(tuán)體標(biāo)準(zhǔn)《含氨基酸水溶肥料游離氨基酸含量的測(cè)定—分光光度法》制定項(xiàng)目由廣西肥料協(xié)會(huì)歸口，項(xiàng)目周期為6個(gè)月，完成年限為2022年12月，標(biāo)準(zhǔn)起草單位為：廣西壯族自治區(qū)分析測(cè)試研究中心、廣西樂(lè)土生物科技有限公司、廣西垂青生物科技有限公司、廣西壯族自治區(qū)地質(zhì)礦產(chǎn)測(cè)試研究中心、廣西壯族自治區(qū)產(chǎn)品質(zhì)量檢驗(yàn)研究院、廣西西大檢測(cè)有限公司等。1.2項(xiàng)目概況現(xiàn)有國(guó)家標(biāo)準(zhǔn)推薦使用的兩種游離氨基酸檢測(cè)方法，所使用的儀器價(jià)格昂貴（自動(dòng)分析儀每臺(tái)80萬(wàn)元以上，液相色譜儀及配套儀器10萬(wàn)元以上），標(biāo)準(zhǔn)溶液價(jià)格也很貴,檢測(cè)成本高，而且檢測(cè)周期長(zhǎng)，結(jié)果滯后，不能及時(shí)指導(dǎo)生產(chǎn)?，F(xiàn)立項(xiàng)研究的《含氨基酸水溶肥料游離氨基酸含量的測(cè)定—分光光度法》檢測(cè)成本低，檢測(cè)速度快，非常適合肥料生產(chǎn)工藝的管理和質(zhì)量控制，大大節(jié)省了企業(yè)的成本。1.3承擔(dān)單位情況廣西壯族自治區(qū)分析測(cè)試研究中心（以下簡(jiǎn)稱“中心）為公益二類事業(yè)單位，成立于1978年，是廣西科技廳直屬的以分析測(cè)試技術(shù)研究、理化分析為主的省級(jí)綜合分析測(cè)試研究機(jī)構(gòu)，是廣西質(zhì)量技術(shù)監(jiān)督局授權(quán)建立的“廣西壯族自治區(qū)保健食品及生物產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)站”，屬于為社會(huì)公眾服務(wù)、對(duì)外獨(dú)立開(kāi)展檢驗(yàn)/檢測(cè)業(yè)務(wù)的第三方檢測(cè)研究機(jī)構(gòu)。中心現(xiàn)有職工82人，其中高級(jí)職稱18人，中級(jí)職稱29人，碩士研究生17人，從事質(zhì)檢工作76人。中心擁有固定資產(chǎn)7809萬(wàn)元，儀器設(shè)備1402臺(tái)套，其中50萬(wàn)元以上的大型儀器37臺(tái)套，20萬(wàn)以上儀器92臺(tái)套，如氣相色譜/質(zhì)譜聯(lián)用儀（GC/MS）、液相色譜/質(zhì)譜聯(lián)用儀（LC/MS）、氣相色譜/紅外光譜聯(lián)用儀（GC/RFX）、氨基酸分析儀、全自動(dòng)遺傳分析儀、高效液相色譜儀、全自動(dòng)超高壓液相色譜儀、等離子發(fā)射光譜儀（ICP）、等離子體質(zhì)譜儀(ICP/MS)、離子色譜儀（IC）、X射線熒光光譜儀、原子熒光分光光度計(jì)、原子吸收分光光度計(jì)等。歷年來(lái)中心承擔(dān)多項(xiàng)省部級(jí)重要課題，獲得科技成果27項(xiàng)，其中廣西科技進(jìn)步獎(jiǎng)8項(xiàng)。中心承擔(dān)各類產(chǎn)品質(zhì)量技術(shù)標(biāo)準(zhǔn)的撰寫(xiě)起草工作，其中3項(xiàng)國(guó)家行業(yè)標(biāo)準(zhǔn)、22項(xiàng)廣西地方標(biāo)準(zhǔn)和50項(xiàng)企業(yè)標(biāo)準(zhǔn)已通過(guò)有關(guān)主管部門(mén)認(rèn)可發(fā)布實(shí)施。中心在生物樣品有效成分分析、有益活性菌分析、保健食品功效成份分析、農(nóng)藥殘留、獸藥殘留檢測(cè)等領(lǐng)域處于廣西領(lǐng)先水平。1.4參編單位及主要起草人工作情況廣西壯族自治區(qū)分析測(cè)試研究中心負(fù)責(zé)統(tǒng)一樣品的收集和分發(fā)，分析方法的實(shí)驗(yàn)研究，樣品測(cè)試結(jié)果的收集和處理，標(biāo)準(zhǔn)文本、試驗(yàn)報(bào)告和編制說(shuō)明的撰寫(xiě)。廣西樂(lè)土生物科技有限公司、廣西垂青生物科技有限公司、廣西壯族自治區(qū)地質(zhì)礦產(chǎn)測(cè)試研究中心、廣西壯族自治區(qū)產(chǎn)品質(zhì)量檢驗(yàn)研究院、廣西西大檢測(cè)有限公司方法驗(yàn)證單位，負(fù)責(zé)對(duì)試驗(yàn)報(bào)告中的條件試驗(yàn)進(jìn)行驗(yàn)證，并對(duì)標(biāo)準(zhǔn)文本提出修改意見(jiàn)。標(biāo)準(zhǔn)主要起草人以及分工如表1所示。表1標(biāo)準(zhǔn)主要起草人及分工單位姓名分工廣西壯族自治區(qū)分析測(cè)試研究中心黃一帆、陳桂鸞、潘揚(yáng)昌、李義芬、班雁華、鄧藝萍、黃殿貴、莫達(dá)松、陸云、陸銀英、劉永強(qiáng)、陳海燕、唐小麗、許園園、陳艷、譚燚主起草單位廣西樂(lè)土生物科技有限公司陸明光、呂貴升、鄧多桓、滕麗娜、陳裕新共同起草單位、方法驗(yàn)證廣西垂青生物科技有限公司韋曉社、賈虎成、陳小莉共同起草單位、方法驗(yàn)證廣西壯族自治區(qū)產(chǎn)品質(zhì)量檢驗(yàn)研究院吉日文、陳海艷、陸章權(quán)共同起草單位、方法驗(yàn)證廣西壯族自治區(qū)地質(zhì)礦產(chǎn)測(cè)試研究中心劉輝庭、梁鑫佳、盧一葉共同起草單位、方法驗(yàn)證廣西西大檢測(cè)有限公司周權(quán)能、裴根、李輝寧共同起草單位、方法驗(yàn)證1.5標(biāo)準(zhǔn)起草過(guò)程廣西壯族自治區(qū)分析測(cè)試研究中心接到《含氨基酸水溶肥料游離氨基酸含量的測(cè)定—分光光度法》的制定任務(wù)后，立即組織相關(guān)工程技術(shù)人員成立了標(biāo)準(zhǔn)編制組，進(jìn)行相關(guān)資料的查詢與收集工作，制訂工作計(jì)劃和進(jìn)度安排。編制組首先查閱大量材料，并根據(jù)NY/T1975—2010《水溶肥料游離氨基酸含量的測(cè)定》中自動(dòng)分析儀法（仲裁法）的原理，設(shè)計(jì)出一個(gè)初步的檢測(cè)方案，然后再制定出實(shí)驗(yàn)的每一個(gè)具體操作步驟。通過(guò)大量的實(shí)驗(yàn)，不斷完善實(shí)驗(yàn)步驟，優(yōu)化檢測(cè)方案，然后確定出一個(gè)檢測(cè)結(jié)果穩(wěn)定、操作簡(jiǎn)單的實(shí)驗(yàn)方法，再按照確定的實(shí)驗(yàn)方法進(jìn)行大量的比對(duì)實(shí)驗(yàn)，根據(jù)比對(duì)實(shí)驗(yàn)的統(tǒng)計(jì)結(jié)果確定出一個(gè)矯正系數(shù)。在此基礎(chǔ)上，于2022年10月形成了標(biāo)準(zhǔn)的討論稿和編制說(shuō)明。本標(biāo)準(zhǔn)討論稿完成后，在編制組及單位內(nèi)部進(jìn)行了多次交流，廣泛征求意見(jiàn)，對(duì)本標(biāo)準(zhǔn)討論稿進(jìn)行了認(rèn)真的修改和完善，最后形成了該標(biāo)準(zhǔn)的征求意見(jiàn)稿。標(biāo)準(zhǔn)的制訂原則、主要內(nèi)容與論據(jù)2.1標(biāo)準(zhǔn)編制的原則該標(biāo)準(zhǔn)按照GB/T1.1—2020《標(biāo)準(zhǔn)化工作導(dǎo)則第1部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》的規(guī)定和要求編寫(xiě)。本文件堅(jiān)持以生產(chǎn)實(shí)際的可操作性為前提，以滿足其實(shí)踐性、適應(yīng)性、便捷性等需要為原則。2.2確定標(biāo)準(zhǔn)的主要內(nèi)容2.2.1標(biāo)準(zhǔn)題目與用途本文件的立項(xiàng)名稱為：“含氨基酸水溶肥料游離氨基酸含量的測(cè)定—分光光度法”，在標(biāo)準(zhǔn)征求意見(jiàn)的過(guò)程中未提出其他建議，確定為此項(xiàng)標(biāo)準(zhǔn)的名稱。本標(biāo)準(zhǔn)規(guī)定了水溶肥中游離氨基酸含量測(cè)定的分光光度法的試驗(yàn)方法。本標(biāo)準(zhǔn)適用于液體或固體水溶肥料中游離氨基酸含量的測(cè)定。2.2.2試劑表1所需試劑名稱規(guī)格所需濃度亮氨酸99%240mg/L茚三酮分析純3%異丙醇分析純10%抗壞血酸分析純0.8g/L鹽酸分析純0.06mol/L乙二胺四乙酸二鈉分析純10g/L冰乙酸分析純/乙酸鈉分析純/活性炭分析純/2.2.3設(shè)備分光光度計(jì)、分析天平2.2.4試驗(yàn)步驟2.2.4.1試樣的制備固體樣品經(jīng)多次縮分后，取出約100g，將其迅速研磨至全部通過(guò)0.50mm孔徑篩（如樣品潮濕，可通過(guò)1.00mm篩子），混合均勻，置于潔凈、干燥容器中。液體樣品經(jīng)多次搖動(dòng)后，迅速取出約200mL，置于潔凈、干燥的容器中。2.2.4.2試樣溶液的制備稱取試樣1g～5g（精確到0.001g），置于250mL容量瓶中，用水充分溶解后定容到刻度，搖勻后干過(guò)濾，棄去20mL初濾液。取約30mL濾液于小燒杯中，加入一勺（約2g）活性炭攪拌2min，靜置5min后干過(guò)濾，再用0.45微米的微孔濾膜過(guò)濾濾液。準(zhǔn)確移取0.50mL濾液于50mL容量瓶中，加入1.0mLEDTA-Na溶液（3.2.3）和1.0mL鹽酸溶液（3.2.1），用酸-乙酸鈉緩沖溶液定容，搖勻后干過(guò)濾，濾液備用待測(cè)。2.2.4.3標(biāo)準(zhǔn)曲線的繪制空白溶液的制備：用移液管依次吸取2.00mL蒸餾水、1.00mL茚三酮溶液、0.50mL抗壞血酸溶液、1.50mL乙酸-乙酸鈉緩沖溶液于具塞比色管中，在100℃的沸水中加熱15min，取出冷卻至室溫，搖勻。標(biāo)準(zhǔn)曲線的繪制：用移液管吸取1.00mL、2.00mL、3.00mL、4.00mL氨基酸標(biāo)準(zhǔn)溶液分別置于4個(gè)50mL容量瓶中，用10%異丙醇溶液定容，搖勻。分別用移液管依次吸取2.00mL上述溶液、1.00mL茚三酮溶液、0.50mL抗壞血酸溶、1.50mL乙酸-乙酸鈉緩沖溶液于具塞比色管中，在100℃的沸水中加熱15min，取出冷卻至室溫，搖勻。以空白溶液為參比，于波長(zhǎng)573nm出測(cè)定各吸光度。以氨基酸標(biāo)準(zhǔn)溶液的濃度為縱坐標(biāo)，吸光度為橫坐標(biāo)繪制標(biāo)準(zhǔn)曲線。2.2.4.4樣品的測(cè)定分別用移液管依次吸取2.00mL試樣溶液（3.4.2）、1.00mL茚三酮溶液、0.50mL抗壞血酸溶液、1.50mL乙酸-乙酸鈉緩沖溶液于具塞比色管中，在100℃的沸水中加熱15min，取出冷卻至室溫，搖勻。以空白溶液為參比，于波長(zhǎng)573nm處測(cè)定樣品溶液吸光度，在標(biāo)準(zhǔn)曲線上查得相應(yīng)的游離氨基酸質(zhì)量。2.3主要試驗(yàn)驗(yàn)證情況（1）為驗(yàn)證本文件測(cè)試方法的適用性，由廣西壯族自治區(qū)分析測(cè)試研究中心提供代表性的含氨基酸水溶肥料樣品，統(tǒng)一分配樣品并安排驗(yàn)證試驗(yàn)。除了使用分光光度法進(jìn)行測(cè)試以外，廣西壯族自治區(qū)分析測(cè)試研究中心還使用國(guó)標(biāo)法—高效液相色譜法進(jìn)行測(cè)試。各驗(yàn)證實(shí)驗(yàn)室將分光光度法的值與高效液相法的值相除即可得到矯正系數(shù)f，然后使用統(tǒng)計(jì)學(xué)原理—格拉布斯檢驗(yàn)法對(duì)f進(jìn)行評(píng)價(jià)，評(píng)判最小值或最大值是否離群。表2驗(yàn)證試驗(yàn)數(shù)據(jù)樣品編號(hào)系數(shù)f平均值標(biāo)準(zhǔn)偏差相對(duì)標(biāo)準(zhǔn)偏差%最小值最大值GminGmax實(shí)驗(yàn)室1實(shí)驗(yàn)室2實(shí)驗(yàn)室3實(shí)驗(yàn)室42207012.082.061.961.851.990.115.31.852.081.290.872207022.011.982.042.002.010.021.21.982.041.121.262207031.951.922.011.961.960.042.01.922.011.141.282207041.851.821.771.921.840.063.51.771.921.161.242207051.571.611.511.601.570.053.01.511.611.410.762207061.531.571.441.501.510.053.61.441.571.241.152207071.761.811.691.611.720.095.11.611.811.221.062207081.481.421.451.511.460.042.81.421.511.111.232207091.621.581.671.591.620.042.51.581.670.921.332207101.771.811.791.851.810.031.81.771.850.961.312207111.531.511.441.351.460.085.71.351.531.350.842207121.931.841.891.781.860.063.51.781.931.241.082207131.851.871.941.921.890.042.21.851.941.151.062207141.811.851.771.671.780.084.31.671.851.370.982207152.082.082.042.162.090.052.32.042.160.921.422207162.031.981.901.961.960.052.81.902.031.251.152207171.401.481.441.561.470.074.51.401.561.071.302207181.441.391.501.501.460.053.81.391.501.290.792207192.292.202.182.452.280.125.52.182.450.841.372207202.122.002.001.882.000.104.81.882.121.221.222207211.411.451.511.591.490.085.21.411.591.011.292207221.381.421.491.341.410.064.51.341.491.051.282207231.941.881.821.741.850.094.61.741.941.221.092207241.811.931.981.851.890.073.91.811.981.071.1422072512.7512.1912.6312.0012.390.352.912.0012.751.101.012207262.632.542.792.712.670.114.02.542.791.161.162207272.071.971.901.941.970.073.81.902.071.001.362207282.152.212.062.012.110.094.12.012.211.101.152207292.202.132.002.102.110.084.02.002.201.311.102207301.942.031.861.771.900.115.91.772.031.191.162207312.091.962.062.262.090.126.01.962.261.071.332207322.252.152.061.972.100.125.71.972.251.141.182207332.312.292.292.252.280.021.12.252.311.450.842207341.601.571.521.461.540.064.01.461.601.271.052207351.401.441.441.481.440.032.21.401.481.171.28220400253.763.643.713.953.760.133.53.643.950.941.39220401924.114.023.953.843.980.112.93.844.111.221541.521.631.541.560.053.31.521.630.761.47220403603.433.563.503.313.450.113.13.313.561.301.04220407281.801.851.751.641.760.094.91.641.851.351.00220500571.571.551.481.431.510.064.11.431.571.200.99220502084.724.824.714.654.730.071.44.654.821.061.35220509451.641.561.521.701.610.084.91.521.701.051403.503.563.503.490.071.93.403.561.371.03220514811.691.631.571.661.640.053.11.571.691.251.11220603473.483.573.463.863.590.185.13.463.860.731.45220500231.381.461.421.561.460.085.51.381.560.931.38220500241.691.731.901.891.800.115.91.691.901.010.90220500251.511.531.401.651.520.106.61.401.651.181.26220500261.591.521.461.521.520.063.61.461.591.191.26220501932.001.981.901.821.920.084.41.822.001.280.94220501941.841.911.931.951.900.052.51.841.951.410.89220501951.951.921.861.851.890.052.61.851.950.981581.641.721.641.650.053.31.581.721.101.32220104761.551.541.591.671.590.063.61.541.670.811.41220106702.302.272.272.222.260.031.42.222.301.351.06220305202.832.882.792.882.840.041.42.792.881.310.78220305264.254.554.554.854.550.245.44.254.851.221.22220307092.032.082.152.352.150.146.62.032.350.871.40220307102.092.132.132.202.140.052.12.092.201.041.36220313642.352.352.402.602.430.124.92.352.600.631.47220603472.262.322.372.532.370.124.92.262.530.951.38220305263.353.253.253.553.350.144.23.253.550.711.41220705821.791.771.761.811.780.021.31.761.810.911.28220711133.002.832.802.652.820.145.12.653.001.181.26220712691.962.052.122.242.090.125.61.962.241.131.25220712702.142.202.332.392.260.115.02.142.391.081.08220713082.042.011.972.042.010.031.61.972.041.340.83220713092.102.012.072.082.070.041.72.012.101.430.89220816931.961.891.942.001.950.052.41.892.001.281701.781.831.851.790.073.71.701.851.330.86格拉布斯檢驗(yàn)結(jié)果表明測(cè)定結(jié)果中無(wú)異常值（當(dāng)n=4，α=0.05時(shí)臨界值為1.481，α=0.01時(shí)臨界值為1.496）。各實(shí)驗(yàn)室試驗(yàn)數(shù)據(jù)表3實(shí)驗(yàn)室一試驗(yàn)數(shù)據(jù)樣品編號(hào)氨基酸含量（%）液相法%系數(shù)f測(cè)定值1測(cè)定值2平均值相對(duì)偏差22070115.2913.6714.485.66.962.0822070226.6424.9325.783.312.812.0122070323.3922.2922.842.411.691.9522070417.8516.9217.392.79.381.8522070516.3217.8917.114.610.881.5722070613.0014.3513.674.98.971.5322070714.1113.2813.703.07.771.7622070814.0512.6713.365.29.051.4822070925.8324.0824.963.515.371.6222071024.6023.4524.032.413.541.7722071111.2210.3610.794.07.061.5322071218.6020.6119.605.110.161.9322071320.6422.0021.323.211.551.8522071421.1820.4920.841.711.521.8122071522.2521.0021.632.910.422.0822071625.9723.7424.854.512.262.032207179.249.299.270.36.631.4022071810.6711.4211.043.47.671.442207190.450.410.434.20.192.292207200.550.600.583.90.272.1222072110.809.9610.384.07.351.4122072213.2414.1013.673.19.901.3822072317.0415.1316.095.98.291.9422072416.8518.4317.644.59.721.812207258.8910.009.455.90.7412.752207263.002.732.864.81.092.6322072718.7120.5119.614.69.472.0722072823.5521.3822.464.810.472.1522072925.3224.3124.822.011.282.2022073015.6414.1714.914.97.681.9422073117.0918.6317.864.38.552.0922073222.6921.5422.112.69.842.2522073324.6726.1725.422.911.032.3122073422.7024.6123.664.014.781.6022073518.4517.1817.823.612.731.40220400259.3810.099.733.72.593.762204019230.5732.6031.593.27.694.112204023628.4330.3329.383.219.091.54220403602.292.142.213.30.653.43220407289.429.179.301.35.181.802205005725.0323.2924.163.615.401.572205020838.1734.5836.374.97.714.722205094515.1213.6414.385.28.761.642205143726.6729.9228.295.78.333.402205148121.2120.5320.871.612.331.692206034716.6215.5016.063.54.613.482205002316.3915.0815.744.211.391.382205002415.9017.3816.644.49.841.692205002517.4217.0317.231.111.411.512205002618.3216.4717.395.310.921.592205019331.9129.0430.484.715.222.002205019427.8627.0627.461.514.961.842205019530.3527.6529.004.614.871.952201047516.6715.2815.984.310.081.582201047616.2614.8015.534.710.001.552201067019.6020.8120.203.08.792.30220305202.943.303.125.91.102.83220305260.350.330.343.50.084.25220307090.370.340.353.70.172.032203071020.7219.4420.083.29.602.09220313642.422.242.333.80.992.352206034710.6310.2310.431.94.612.26220305260.250.280.274.50.083.352207058223.9726.5925.285.214.131.79220711130.580.620.603.30.203.00220712696.426.006.213.43.171.96220712706.386.556.471.33.022.142207130819.0818.3218.702.09.162.042207130917.5018.5018.002.88.582.102208169323.3325.5624.444.512.481.962208169426.6424.2525.444.714.961.70表4實(shí)驗(yàn)室二試驗(yàn)數(shù)據(jù)樣品編號(hào)氨基酸含量（%）液相法%系數(shù)f測(cè)定值1測(cè)定值2平均值相對(duì)偏差22070113.8314.9014.373.76.962.0622070224.2626.4725.374.312.811.9822070321.7823.0522.422.811.691.9222070416.5717.6217.093.19.381.8222070518.1616.8417.503.810.881.6122070614.8813.2714.085.78.971.5722070714.6213.5214.073.97.771.8122070812.2413.4512.844.79.051.4222070924.9623.6124.282.815.371.5822071024.0725.0424.562.013.541.8122071110.1611.2210.694.97.061.5122071218.0019.4218.713.810.161.8422071321.0022.2721.642.911.551.8722071420.8421.8221.332.311.521.8522071522.6720.5821.634.810.422.0822071623.5125.0324.273.112.261.982207179.5710.039.802.36.631.4822071810.0811.1710.635.17.671.392207190.430.390.414.50.192.202207200.530.560.553.30.272.0022072110.2411.0810.663.97.351.4522072214.4813.7114.102.79.901.4222072315.3115.9515.632.08.291.8822072419.6317.8718.754.79.721.932207259.548.529.035.60.7412.192207262.912.642.774.91.092.5422072717.9919.3718.683.79.471.9722072822.2823.9123.103.510.472.2122072924.8623.2124.043.411.282.1322073014.8116.3715.595.07.682.0322073117.0116.4116.711.88.551.9622073221.6920.5921.142.69.842.1522073324.6725.8925.282.411.032.2922073424.1022.1723.134.214.781.5722073517.4519.0918.274.512.731.44220400259.918.939.425.22.593.642204019229.7032.1630.934.07.694.022204023630.5027.5229.015.119.091.52220403602.182.422.305.30.653.56220407289.829.309.562.85.181.852205005723.5724.0523.811.015.401.552205020835.1939.0837.145.27.714.822205094514.3013.0613.684.58.761.562205143728.1730.0829.133.38.333.502205148119.5020.5820.042.712.331.632206034717.3415.5516.455.54.613.572205002317.6215.5716.606.211.391.462205002417.4616.4816.972.99.841.732205002517.9716.8817.423.111.411.532205002615.8817.3116.604.310.921.522205019331.5728.6130.094.915.221.982205019429.9127.1328.524.914.961.912205019526.8730.1728.525.814.871.922201047517.3215.7716.544.710.081.642201047614.3916.4215.416.610.001.542201067020.5619.2719.923.28.792.27220305203.033.303.174.31.102.88220305260.380.340.365.50.084.55220307090.370.360.361.20.172.082203071021.2819.6020.444.19.602382.282.332.10.992.352206034711.1710.2310.704.44.612.32220305260.250.270.264.60.083.252207058226.2723.6524.965.214.131.77220711130.560.570.570.90.202.83220712696.836.176.505.13.172.05220712706.476.816.642.63.022.202207130817.8218.9918.403.29.162.012207130916.9217.6717.292.28.582.012208169322.5624.5323.554.212.481.892208169425.4927.6126.554.014.961.78表5實(shí)驗(yàn)室三試驗(yàn)數(shù)據(jù)樣品編號(hào)氨基酸含量（%）液相法%系數(shù)f測(cè)定值1測(cè)定值2平均值相對(duì)偏差22070113.1014.1613.633.96.961.9622070227.3224.9426.134.512.812.0422070323.9023.1423.521.611.692.0122070417.1815.9516.573.79.381.7722070515.6117.1916.404.810.881.5122070613.5412.2812.914.98.971.4422070712.7013.5213.113.17.771.6922070813.3612.8413.102.09.051.4522070924.7226.6225.673.715.371.6722071024.8723.5424.202.713.541.792207119.6310.7610.205.57.061.4422071218.6219.7819.203.010.161.8922071321.5523.1822.363.711.551.9422071421.4119.4520.434.811.521.7722071522.1720.4221.294.110.422.0422071624.2722.2423.264.412.261.902207179.399.759.571.96.631.4422071812.0011.0011.504.37.671.502207190.390.420.413.40.192.182207200.520.570.555.00.272.0022072111.6310.5211.085.07.351.5122072215.1414.3814.762.69.901.4922072315.6814.4915.083.98.291.8222072418.8019.6319.212.29.721.982207258.989.729.354.00.7412.632207263.182.913.054.51.092.7922072718.6817.2217.954.19.471.9022072820.5722.6521.614.810.472.0622072922.0223.0322.522.211.282.0022073014.8113.8114.313.57.681.8622073118.3816.7517.564.68.552.0622073220.9619.5020.233.69.842.0622073325.8924.6725.282.411.032.2922073423.2221.7322.473.314.781.5222073519.0017.5518.274.012.731.442204002510.009.209.604.22.593.712204019230.7529.9330.341.47.693.952204023632.0730.3331.202.819.091.63220403602.182.342.263.60.653.50220407289.478.689.084.35.181.752205005723.7321.9022.824.015.401.482205020837.6335.0436.343.67.714.712205094512.6414.0513.355.38.761.522205143730.5028.7529.633.08.333.562205148120.0818.7519.423.412.331.572206034716.0915.7815.941.04.613.462205002316.3915.9016.151.511.391.422205002419.1818.1118.652.99.841.902205002516.8015.2316.024.911.411.402205002616.8115.0415.925.510.921.462205019330.2627.5728.914.715.221.902205019427.9129.7428.833.214.961.932205019528.9626.3527.654.714.871.862201047516.6717.9717.323.810.081.722201047616.3415.3715.853.110.001.592201067019.6020.3219.961.88.792.27220305203.123.033.071.51.102.79220305260.370.350.363.30.084.55220307090.360.390.374.70.172.152203071021.1219.8420.483.19.602482.282.384.20.992.402206034711.4110.4710.944.34.612.37220305260.260.250.261.50.083.252207058223.7326.0324.884.614.131.76220711130.530.590.565.40.202.80220712697.006.426.714.33.172.12220712706.817.247.033.13.022.332207130817.4818.6618.073.39.161.972207130917.5018.0817.791.68.582.072208169324.9623.5024.233.012.481.942208169426.4628.4127.433.514.961.83表6實(shí)驗(yàn)室四試驗(yàn)數(shù)據(jù)樣品編號(hào)氨基酸含量（%）液相法%系數(shù)f測(cè)定值1測(cè)定值2平均值相對(duì)偏差22070113.5912.2012.895.46.961.8522070224.4326.8125.624.612.812.0022070322.3723.5622.972.611.691.9622070418.5817.4518.023.29.381.9222070516.6718.2517.464.510.881.6022070612.8213.9913.404.38.971.5022070713.1611.8812.525.17.771.6122070814.3113.1013.714.49.051.5122070925.4323.5324.483.915.371.5922071025.8424.2525.043.213.541.852207119.969.049.504.97.061.3522071218.9817.1918.094.910.161.7822071321.3622.9122.143.511.551.9222071418.6319.8619.243.211.521.6722071521.6723.2522.463.510.422.1622071624.5223.4223.972.312.261.9622071710.4910.1210.311.86.631.5622071812.0810.9211.505.17.671.502207190.440.480.464.10.192.452207200.530.500.512.70.271.8822072112.0111.3611.682.87.351.5922072213.7112.8613.293.29.901.3422072314.9513.9414.453.58.291.7422072418.8017.2218.014.49.721.852207259.268.528.894.20.7412.002207262.823.092.954.61.092.7122072717.4719.2818.384.99.471.9422072822.0120.1221.074.510.472.0122072924.1323.3023.721.711.282.1022073014.1712.9913.584.47.681.7722073118.8919.6619.272.08.552.2622073220.1418.5919.364.09.841.972207