GXASI本文件參照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1水牛乳中類固醇激素類藥物多殘留量的測(cè)定液相色譜-串聯(lián)質(zhì)譜法本文件規(guī)定了水牛乳中13種類固醇激素類藥物多殘留量的液相色譜-串聯(lián)質(zhì)GB/T6682分析實(shí)驗(yàn)室用水規(guī)格GB/T27404實(shí)驗(yàn)室質(zhì)量控制規(guī)范食品理化4試劑與材料）：）：）：）：4.2試劑配制4.3標(biāo)準(zhǔn)品24.4標(biāo)準(zhǔn)溶液配制4.4.1標(biāo)準(zhǔn)儲(chǔ)備液：分別稱取適量（精確至0.00001g）各標(biāo)4.4.2混合標(biāo)準(zhǔn)中間液：分別準(zhǔn)確移取適量的異氟潑尼松、鹵米松、氟尼縮松、地索奈德、睪酮、美），4.5材料4.5.2聚丙烯離心管：15mL，50mL。5.1液相色譜-串聯(lián)質(zhì)譜儀，配有電噴霧離子源（ESI從所取全部樣品中取出有代表性樣品約500g，充分搖勻，均分成兩份，分別裝入潔凈容器中，密封，并標(biāo)明標(biāo)記。將試樣置于0℃~4℃冷藏存放。稱取2g（精確至0.01g）混合均勻的樣品，置于50mL離心管中，分別加入5.0mL水和10.0mL乙腈，渦旋提取10min，加入亞鐵氰化鉀溶液（4.2.1）和乙酸鋅溶液（4.2.2）各0.2mL，渦旋5min，加入），取2mL上清液轉(zhuǎn)移至凈化管（分別稱取0.15gMgSO4、0.10gPSA、0.10gC18至15mL離心管中）中，渦旋1min，10000r/min離心5min。準(zhǔn)確吸取1mL上清液于40℃下用氮?dú)獯蹈桑詈笥?.3A/%B/%08h）13種類固醇激素類藥物的監(jiān)測(cè)離子對(duì)參數(shù)47.3.2.2按照上述條件測(cè)定樣品和標(biāo)準(zhǔn)工作液，如果檢測(cè)的質(zhì)量色譜峰保留時(shí)間與標(biāo)準(zhǔn)工作液的色譜峰保留時(shí)間偏差在±2.5％之內(nèi)；定性離子對(duì)的相對(duì)豐度與相當(dāng)濃度的標(biāo)準(zhǔn)工作液的相對(duì)豐度一致，相>50%>2050%>1020%≤10%±20%±25%±30%±50%液相色譜-串聯(lián)質(zhì)譜法測(cè)定采用標(biāo)準(zhǔn)曲線法定量X——試樣中目標(biāo)化合物的殘留量的質(zhì)量分?jǐn)?shù)，單位為微克每千克(μg/kgc——由回歸曲線計(jì)算得到的上機(jī)試樣溶液中目標(biāo)化合物的濃度，單位為微克每升(V——濃縮至干后試樣的定容體積，單位為毫升（f——稀釋倍數(shù)；注：計(jì)算結(jié)果應(yīng)扣除空白值，測(cè)定結(jié)果用平行測(cè)定的算5metandienonemegestrolacetatemedroxyprogesterone17-acetatehydroxyprogesteronecap678表C.1給出了13種類固醇激素類藥物測(cè)定的添加回收回收率/%相對(duì)標(biāo)準(zhǔn)偏差RSD/%70.3105.3%110.0118.0%70.489.8%72.396.8%72.494.3%81.389.4%70.488.7%72.578.5%82.787.0%88.398.8%77.8110.2%75.679.1%86.497.9%79.3103.1%80.898.2%80.6110.5%82.1109.7%78.091.1%72.4110.2%72.086.7%73.283.2%70.484.8%74.081.5%75.980.5%70.188.8%73.593.5%71.482.5%70.781.7%71.6106.1%70.472.3%74.480.8%80.099.2%75.289.3%70.181.5%76.1112.1%79.380.5%83.190.3%70.781.6%72.379.8%82.086.8%78.083.2%85.694.2%83.988.7%77.283.9%79.694.2%84.791.5%84.791.5%86.998.7%81.584.3%81.584.3%98.3108.5%80.687.2%80.687.2%88.599.3%93.5107.3%82.098.8%76.379.8%92.494.8%83.690.7%87.3108.0%91.993.5%80.989.4%77.290.3%85.1102.0%73.689.3%72.889.6%84.789.2%74.081.1%71.988.0%84.691.1%76.480.6%75.680.3%72.295.1%77.190.2%74.385.4%82.390.4%74.079.5%70.594.3%78.283.1%71.275.8%70.880.2%82.595.5%70.483.9%74.379.8%86.890.8%75.283.9%70.385.4%88.693.5%77.282.3%77.491.7%81.594.3%72.678.0%72.780.1%80.087.0%73.276.0%70.878.5%83.189.5%73.076.3%72.380.2%78.7115.3%100.8114.9%74.195.9%75.484.0%73.181.2%85.4101.7%82.191.1%70.779.0%74.995.2%71.17