饲料中β-受体激动剂的测定 液相色谱-串联质谱法 编制说明_第1页
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(一)任务来源 1(三)起草过程 7 7(三)主要技术内容的确定依据 17 (一)方法学考察 19 44 1一、工作简况近年来,食品安全问题已成为社会普遍关心的热点话题,习总书记对食品近年媒体曝光了许多畜产品质量安全问题,其中2009年的雨润、2011年的双汇、2015年的金锣火腿均被查出掺杂各类“瘦肉精”。2020年,山东、2去甲肾上腺素的一大类化合物统称,临床上常被用来治疗人的呼吸系统疾病。常被不法分子作为饲料添加剂用于畜禽养殖。动物食用含β-受体激动剂的饲3精,远不能满足目前监管需要。此外2006版标准的测定方法为高效液相色谱-受体激动剂测定方法的兼容性,以提高检测效率,易于方法的推广普及。本4激动剂的方法标准(不含修订的2项标准),见表3。为尽量扩大新方法的检1234饲料中22种β-受体激动剂的测定液相色谱-串联质谱法55123456789猪毛中7种β–受体激动剂残留量的测定液相色谱–串联质6总共发送“征求意见稿”25份,回函20份,合并相同意见后共计52条,7二、标准编制原则、主要内容及其确定依据本标准的结构、技术要素及表述形式按照GB/T1.1-2020《标准化工作导4部分:试验方法标准》的规定和要求进行编写。根据国内外检测技术发展趋8为保障饲料产品质量安全,满足管理部门监管需要,收集整理现有饲料、用性,在确保方法准确性和灵敏度的前提下,本次修订将检测参数扩大至21120189-2006)23乙酸钠缓冲液(pH4.8)40.1mol/L盐酸+甲醇=80+20;饱50.1mol/L盐酸+甲醇=80+20;饱60.1mol/L盐酸+7乙酸铵溶液、高9液相色谱-串联质谱法(NY/T3144-2017)“瘦肉精”是一类具有促进蛋白质合成,抑制脂肪沉积的苯乙醇胺类化合物的统称。它们同属于肾上腺素受体(主要为β受体)激动剂类物质,按结构通常可分为苯胺型、苯酚型和苯二酚型等三大类,均为白色至类白色结晶粉末,料、仔猪配合饲料作为空白基质,添加21种待测物标准溶液,制成添加浓度综上所述,样品提取条件确定如下:平行做两份试验。称取试样2g(精饲料产品基质复杂,除含有植物性、动物性及矿物性等物质外,生产时往根据“瘦肉精”类化合物的理化性质可知,其为碱性化合物,分子结构),氨基与氢离子结合,形成带正电荷的阳离子,其与MCX柱填料上的特征官能将猪配合饲料、鸡浓缩饲料、牛精料补充料作为空白基质,加标制成浓考虑到MCX柱的普及性和成本,试验最终选择规格为60mg/3mL的净化柱。微量元素分别添加成50μg/kg,加入提取液,一份提取液采用MCX柱净化,一份过滤膜,分别上机测定其回收率和精密度。结果表明,经MCX柱净抽干,用5mL5%氨水甲醇溶液洗脱,收集洗脱液,于50℃氮吹至干,准确本试验采用实验室最为常用的C18色谱柱进行优化。试验中分别选用柱长100漂移的影响,试验对柱温也进行了优化。色谱条件的优化既满足了23种待测5555b)脱溶剂气、锥孔气、碰撞气均为高纯气体及其他合适气体,调节各气c)毛细管电压、锥孔电压、碰撞能量等d)定性离子对、定量离子对及对应的保留时间、试验采用安捷伦公司液质联用仪,型号为1290-6495,经各参数优化后其15238456788966饲料、食品、进出口领域的现行标准均对待测“瘦肉精”类化合物的有效规范食品理化检测》中对标准物质有效期的规定[22],并以有证标准溶液的有效期为依据,确定本方法的标准物质有效期。将标准储备液(1mg/mL)及标本次修订重点是规范性要素的选择,尤其是核心技术要素的确定,优化搭总计21种物质,既满足了当前行业需要,也保证了标准的适度前瞻性。标准检测能力的增强可有效震慑饲料中非法添加行为,为产程基本一致,使新旧标准有效衔接,更加便三、试验验证的分析、技术指标论证饲料样品种类繁多基质复杂,其含有的动物蛋白、植物色素等成分往往对待测物的检测产生明显干扰,这些影响被称为基质效应(MatrixEffect是配标准曲线和溶剂标准曲线的比值进行判定。计算公式为ME(%)=B/A×100%,其中A为纯溶剂的标准曲线斜率,B为基质溶液的标准曲线斜率。若结果的准确性。表11给出了乳猪配合饲料和猪复合预混料两类样品的基质效质效应不明显,其余物质均呈现基质增强或目前,基质效应消除方法中应用最多的是基质加标法、基质稀释法及同位y=1831.0x+1764.7,R=0.y=1494.3x+727.6,R=0y=1025.2x+1458.4,R=0.y=1901.5x+789.6,R=0y=3282.3x+11242.9,R=0.9y=2351.2x+3025.9,R=0.y=3159.0x+6987.0,R=0.y=3826.0x+6513.0,R=0.y=3535.5x+4780.1,R=0.y=1458.5x+2499.0,R=0.y=1458.5x+389.0,R=0y=2409.4x+6607.6,R=0.y=1218.3x+3006.6,R=0.y=1467.1x+2235.0,R=0.y=1467.1x+2235.0,R=0.y=3241.8x+2476.2,R=0.y=3982.4x+1783.6,R=0.y=3610.6x-1244.0,R=0.y=1824.3x+1296.6,R=0.y=8313.6x+26986.2,R=0.9y=5475.6x+9589.2,R=0.y=2848.8x+885.0,R=0y=3250.6x+13124.1,R=0.9y=1754.4x-5471.7,R=0.y=1367.4x+3296.1,R=0.y=2251.9x+7756.4,R=0.y=1973.0x+5535.9,R=0.y=3473.6x-806.6,R=0y=5088.5x+7896.0,R=0.y=3433.4x+2465.0,R=0.y=5199.9x+3315.3,R=0.y=6783.2x+11289.2,R=0.9y=5577.4x+11507.5,R=0.9y=2559.8x+3236.8,R=0.y=3587.4x+4989.6,R=0.y=2736.6x+9484.8,R=0.y=1672.2x+2349.5,R=0.y=2651.4x+4553.7,R=0.y=2131.4x+3642.1,R=0.y=3206.2x+7946.4,R=0.y=3967.7x+6547.0,R=0.y=4399.2x+8015.3,R=0.y=24115.1x+18013.6,R=0.9985y=24640.0x+38035.3,R=0.9931y=7173.2x+13363.7,R=0.9y=9199.9x+28501.2,R=0.9y=6530.1x+29743.7,R=0.9y=2147.9x+834.9,R=0y=2026.3x+2580.5,R=0.y=2026.3x+2580.5,R=0.y=2810.8x+5157.8,R=0.y=2591.5x+10478.9,R=0.9y=2903.4x+10138.0,R=0.9y=3035.9x+11314.3,R=0.9y=4880.7x+9723.2,R=0.y=4830.9x+9611.9,R=0.y=7321.5x+20873.2,R=0.9y=8692.8x+25764.4,R=0.9y=9330.5x+13377.7,R=0.9y=1859.2x+1771.9,R=0.y=1638.4x+1638.4,R=0.y=1480.3x+1162.3,R=0.y=8616.7x+22363.3,R=0.9y=12818.8x+14423.4,R=0.9984y=2210.2x+5582.2,R=0.y=2492.3x+8148.2,R=0.y=2302.8x+7287.5,R=0.10ng/mL、25ng/mL、50ng/mL、100ng/mL系列基质标准溶液或双平行单280为基准,计算出萃取柱的离子交换容量(柱容量)约为16.8mg,试验称样量为2g,换算成样品添加浓度为8.4mg/g(含量0.84%)。结合“瘦肉精”添加浓度设定为5μg/g,按优化确定的方法结果显示,23种待测物的回收率均大于60%,证明净化过程中萃取柱填料对待测物有较强的吸附作用,未造成小柱过载现象,测定称取猪配合饲料2g,添加浓度为50μg/kg,选取3个不同厂家的混合型说明不同厂家的固相萃取柱对待测物的净化效果差异不Ci——由基质匹配混合标准曲线查得试样溶液中待测物的浓度,单位);V——试样提取溶液的体积,单位为毫升(mL););f——超出标准曲线后的稀释倍数;Ai——试样溶液中待测物的色谱峰面积;Ais——基质匹配混合标准溶液中待测物的色谱峰面积;Cis——基质匹配混合标准溶液中待测物的浓度,单位为纳克每毫升);V——试样提取溶液的体积,单位为毫升(mL););m——试样质量,单位为克(g)。测定结果以平行测定的算术平均值表示,保留3位有效数字。浓度,即定量限浓度,2倍定量限浓度和5倍定量限浓度,每个添加浓度制备化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5090.786.979.785.382.985.14.182.089.388.384.686.386.12.950079.182.281.882.185.182.12.1特布他林5065.468.972.566.564.967.672.375.471.666.870.271.350074.678.476.171.870.674.33.2沙丁胺醇92.689.482.790.189.388.83.72076.486.283.982.981.182.13.778.579.685.488.684.383.34.2齐帕特罗5089.780.077.484.280.682.44.877.388.478.085.978.981.750081.879.388.387.685.184.43.8西马特罗5094.485.591.581.685.787.75.291.987.081.585.184.386.03.950084.680.581.186.984.783.62.7西布特罗5091.280.784.788.182.685.54.290.885.683.184.388.886.53.250090.685.684.682.689.986.73.5利托君5098.491.890.095.491.693.43.498.395.587.689.994.96.350091.991.192.690.894.992.3克伦塞罗5094.496.086.688.189.290.94.199.689.591.095.595.75.650088.287.684.692.694.189.43.9克伦普罗5072.274.878.873.380.976.03.771.480.187.072.978.578.06.250078.872.975.380.678.577.2氯丙那林5067.566.866.263.364.965.767.063.662.868.971.066.73.550067.166.568.471.266.668.02.0妥布特罗5068.563.869.371.169.968.52.875.873.074.375.174.374.550064.365.070.369.974.368.74.1盐酸克伦特罗65.069.474.772.574.671.24.12075.583.776.688.378.880.65.370.775.378.080.685.578.05.5盐酸溴代克伦特罗5083.176.884.288.685.383.64.382.485.884.381.284.683.750076.476.379.584.182.279.73.5溴布特罗5072.971.871.678.969.773.03.573.475.078.568.970.573.33.850068.866.478.575.271.172.04.8班布特罗5088.182.789.687.186.186.72.689.089.489.790.285.188.72.050080.292.291.084.485.186.65.0盐酸苯氧丙酚胺5096.093.488.082.185.789.05.686.580.985.384.387.684.92.650079.873.179.780.578.178.23.0莱克多巴胺71.482.673.767.272.373.45.62091.393.787.996.376.589.17.780.285.385.582.588.484.4羟甲基克伦特罗5081.267.370.382.970.274.47.181.076.267.577.180.876.55.550073.274.875.185.280.077.74.9盐酸克伦潘特5068.765.565.672.561.466.74.168.172.278.671.061.170.26.450067.068.572.478.570.471.44.5马布特罗5079.774.371.076.371.374.53.776.380.979.383.175.579.03.250065.971.171.968.272.970.02.9盐酸马喷特罗5071.973.180.568.882.375.35.871.082.177.481.667.075.86.650069.666.072.675.570.470.83.5化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5074.371.966.870.578.872.54.567.269.971.074.472.671.02.750065.668.862.270.668.867.23.3特布他林5076.467.372.975.572.272.83.665.270.876.268.267.769.64.250068.278.275.567.971.972.34.5沙丁胺醇66.970.168.268.972.669.32.12062.565.367.268.272.167.13.672.262.964.666.868.266.93.6齐帕特罗5074.471.676.975.568.573.43.367.173.579.270.568.271.74.950068.470.665.176.673.370.84.4西马特罗5084.975.888.182.278.181.85.071.673.574.478.482.476.14.350077.078.969.782.074.376.44.7西布特罗5062.460.569.865.272.266.04.969.965.866.172.463.867.63.550064.870.563.869.572.268.23.7利托君5079.995.193.688.984.688.46.382.684.296.590.282.187.16.250079.381.074.582.683.780.23.6克伦塞罗5085.082.282.986.980.583.52.583.482.289.085.490.586.13.650082.177.478.184.985.681.63.8克伦普罗5078.773.974.180.279.377.33.074.872.982.278.882.978.34.450072.170.168.180.675.573.34.9氯丙那林5079.972.073.571.880.575.54.369.872.263.168.875.269.84.550070.469.865.666.475.469.53.9妥布特罗5066.668.770.569.468.168.772.271.963.172.268.869.63.950069.566.663.967.470.467.62.5盐酸克伦特罗67.572.280.178.874.674.62069.175.265.574.975.472.04.579.875.778.377.780.578.4盐酸溴代克伦特罗5062.967.566.266.871.166.92.964.467.970.572.264.968.03.450078.773.070.473.464.672.0溴布特罗5067.172.473.571.868.870.72.762.868.668.270.075.569.04.550072.168.665.772.466.869.13.0班布特罗5088.893.295.485.984.389.54.780.486.078.687.590.284.54.950072.677.574.484.685.578.95.9盐酸苯氧丙酚胺5092.288.587.089.584.288.33.082.274.581.978.988.781.25.250084.178.978.090.184.683.14.9莱克多巴胺77.380.771.374.472.675.33.82070.669.472.868.975.571.42.777.679.779.478.880.579.2羟甲基克伦特罗5071.574.174.781.071.174.54.066.465.468.668.572.468.32.750067.265.470.174.368.169.03.4盐酸克伦潘特5066.471.276.172.264.970.24.573.166.668.971.075.571.03.550074.675.767.177.371.273.24.1马布特罗5065.882.269.878.671.173.56.765.066.376.668.769.569.24.550063.666.566.672.574.368.74.5盐酸马喷特罗5073.466.470.969.964.669.03.568.465.965.266.667.266.750066.764.165.270.572.567.83.6化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5091.686.088.582.381.986.14.179.178.283.785.684.382.23.350076.077.574.982.681.978.63.5特布他林5082.379.676.380.679.279.62.275.969.876.480.276.675.83.850066.862.772.574.970.169.44.8沙丁胺醇85.288.179.785.580.183.73.72083.574.779.884.375.679.64.480.383.681.172.685.580.64.9齐帕特罗5089.386.388.478.280.684.64.972.579.779.485.582.179.84.850074.981.387.478.681.180.74.6西马特罗5082.089.092.285.581.786.14.578.981.381.376.686.881.03.850072.275.573.181.585.677.65.8西布特罗5086.482.583.878.680.182.377.577.683.186.574.179.85.050083.682.588.076.578.281.74.5利托君5080.489.987.390.195.388.65.494.983.982.388.682.186.45.550088.287.491.390.195.490.53.2克伦塞罗5093.784.991.288.686.589.03.675.777.078.285.280.679.33.750082.283.280.689.284.684.03.3克伦普罗5091.075.184.881.179.682.36.086.687.782.978.280.183.14.150071.171.676.578.682.176.04.7氯丙那林5076.173.381.285.576.978.64.863.772.773.569.572.170.34.050064.267.765.675.570.568.74.5妥布特罗5065.166.568.669.272.668.42.963.464.367.069.971.267.23.450072.470.165.675.572.671.23.7盐酸克伦特罗73.784.987.380.178.981.05.32071.768.266.976.880.172.75.680.378.385.676.286.581.44.5盐酸溴代克伦特罗5085.189.480.172.675.680.66.866.662.866.970.275.668.44.850067.880.471.578.275.574.7溴布特罗5080.389.388.575.878.682.582.877.772.281.685.580.050072.079.177.088.074.978.2班布特罗5086.787.693.285.690.288.680.788.186.082.294.386.35.450084.988.984.491.290.788.03.2盐酸苯氧丙酚胺5076.584.479.872.278.678.34.568.866.769.571.675.370.43.350079.581.777.575.482.179.22.8莱克多巴胺77.183.079.285.580.081.03.32081.871.180.276.788.579.76.476.183.375.580.686.480.44.7羟甲基克伦特罗5071.879.975.480.082.177.84.172.468.172.975.580.173.84.450066.771.267.175.680.072.15.7盐酸克伦潘特5075.775.368.271.180.074.04.672.970.466.578.675.272.74.650066.771.267.170.974.170.0马布特罗5082.587.686.380.178.983.13.878.167.474.976.580.075.44.950075.169.969.775.970.272.2盐酸马喷特罗5086.584.290.280.485.585.43.673.581.977.770.975.575.94.250077.078.172.278.681.177.43.3化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5085.294.690.193.692.85.791.696.586.489.284.689.64.750087.582.389.195.184.487.74.9特布他林5068.972.376.567.464.269.94.775.269.266.671.074.671.33.650066.475.377.168.270.071.44.6沙丁胺醇74.577.588.881.572.278.96.62078.490.687.175.584.483.26.277.270.076.682.588.879.07.1齐帕特罗5077.169.070.771.575.572.83.471.176.379.085.281.178.55.350085.077.574.683.380.080.14.2西马特罗5066.173.867.576.885.273.97.774.669.673.982.277.975.64.750096.281.282.384.786.686.26.0西布特罗5081.482.083.276.275.579.73.579.279.279.380.082.280.050079.377.776.184.281.179.7利托君5066.975.263.279.269.270.76.476.267.867.372.580.172.85.550077.976.476.882.270.076.74.4克伦塞罗5067.765.973.080.178.273.06.269.174.267.581.178.274.05.850078.184.577.880.272.678.64.3克伦普罗5064.466.667.972.876.669.74.969.164.565.476.574.570.05.350075.873.067.379.271.073.34.5氯丙那林5065.567.273.274.669.570.03.965.470.072.876.267.570.44.350075.565.066.472.267.569.34.4妥布特罗5067.764.763.775.374.469.25.464.175.375.372.268.971.24.850066.369.168.375.871.170.13.6盐酸克伦特罗65.575.569.571.072.570.83.72069.266.776.573.172.871.73.869.572.775.480.178.975.34.4盐酸溴代克伦特罗5086.590.295.695.67.386.597.489.292.489.290.94.250091.182.589.294.390.089.44.3溴布特罗5071.069.265.674.275.271.03.969.268.278.570.072.071.64.150064.469.567.871.576.870.04.6班布特罗5095.389.488.492.584.290.04.293.989.495.290.193.84.550085.687.488.894.691.189.53.5盐酸苯氧丙酚胺5088.890.294.695.76.793.491.786.790.093.06.350088.395.992.284.992.76.7莱克多巴胺79.572.888.880.284.181.15.92095.287.284.592.092.26.896.697.289.288.694.85.8羟甲基克伦特罗5078.676.881.092.185.582.86.297.695.290.488.694.54.950097.192.291.886.894.392.43.8盐酸克伦潘特5079.175.473.389.284.180.26.594.990.582.285.288.888.34.950083.790.895.986.684.288.2马布特罗5082.183.470.892.186.282.97.893.795.089.988.684.290.34.350098.085.192.196.17.5盐酸马喷特罗5087.472.787.281.179.281.593.485.292.294.66.750098.393.684.690.293.46.3化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5087.585.082.778.275.681.84.975.776.574.778.080.277.02.250077.875.278.571.273.675.33.0特布他林5068.974.269.272.175.972.162.367.170.868.565.966.950072.770.378.677.273.174.43.4沙丁胺醇77.683.575.877.972.677.54.02068.379.382.584.678.478.66.382.781.880.078.185.981.72.9齐帕特罗5081.490.682.578.188.684.25.275.971.376.180.576.876.13.350072.973.681.878.984.178.34.9西马特罗5077.880.280.785.684.081.667.273.372.776.878.873.84.450070.078.377.074.375.875.13.2西布特罗5087.585.386.283.381.084.72.677.378.585.878.682.280.53.550084.390.187.485.788.887.32.3利托君5078.583.482.280.179.480.72.090.293.999.190.792.293.23.650094.898.790.895.696.74.7克伦塞罗5075.273.381.588.184.180.46.275.475.376.180.682.277.93.250083.191.495.488.482.788.25.5克伦普罗5072.668.770.475.670.071.42.778.568.777.772.174.474.34.050066.070.968.469.673.469.72.8氯丙那林5062.866.568.667.263.665.82.566.864.463.475.270.168.04.850069.967.872.271.169.770.1妥布特罗5065.665.764.170.068.966.92.565.769.963.972.268.868.13.350065.162.267.467.669.966.42.9盐酸克伦特罗74.566.267.672.174.170.93.82078.875.469.872.274.674.23.472.174.568.580.074.473.94.2盐酸溴代克伦特罗5066.867.668.070.568.168.265.669.071.471.970.569.72.550072.473.876.075.980.175.62.9溴布特罗5065.671.471.478.874.572.34.864.673.572.375.968.570.94.450084.182.183.678.880.181.72.2班布特罗5085.590.494.284.185.587.94.380.092.187.788.682.486.24.950085.589.383.088.889.187.12.8盐酸苯氧丙酚胺5077.278.578.371.080.277.03.578.067.075.072.284.375.36.550086.389.985.882.180.584.93.7莱克多巴胺72.874.066.468.275.571.43.92074.475.077.681.172.076.03.585.890.484.280.688.185.83.7羟甲基克伦特罗5067.274.173.870.075.172.03.368.863.172.565.668.067.63.550077.580.778.778.580.679.2盐酸克伦潘特5066.270.373.778.871.572.14.668.265.669.374.375.270.54.150073.270.873.678.971.173.53.3马布特罗5072.866.968.272.275.971.23.668.766.469.768.972.269.22.150073.467.567.375.671.571.13.6马喷特罗5060.567.367.466.872.266.84.269.576.367.672.874.672.23.650067.464.569.972.174.369.63.9化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5080.869.165.170.172.571.55.879.584.375.473.370.076.55.650096.292.285.586.792.26.3特布他林5064.066.664.263.770.865.93.066.765.563.171.268.967.150077.875.666.570.069.972.04.6沙丁胺醇66.069.872.672.975.271.33.52068.067.673.978.970.171.74.779.170.978.172.267.973.64.8齐帕特罗5082.373.177.785.572.278.25.871.978.681.775.580.177.63.950079.184.085.675.580.280.94.0西马特罗5080.170.669.476.472.273.74.470.177.780.073.374.875.23.950091.190.088.882.185.687.53.7西布特罗5068.870.068.672.165.669.02.475.680.579.678.884.279.750084.881.480.985.679.982.52.5利托君5074.767.983.480.277.876.85.969.277.980.177.282.277.35.050085.681.084.876.277.080.94.3克伦塞罗5074.767.983.472.280.275.76.269.277.980.175.581.176.84.850085.681.084.872.578.980.65.3克伦普罗5092.095.393.181.688.290.05.486.486.379.975.580.281.74.750083.990.293.186.282.187.14.5氯丙那林5073.275.781.182.672.276.94.768.874.779.969.581.174.85.750082.989.586.478.880.583.64.4妥布特罗5069.275.366.970.265.569.43.869.464.669.475.579.271.65.750097.484.696.990.282.490.36.9盐酸克伦特罗66.672.171.175.669.971.13.32070.568.267.975.572.170.890.180.580.478.585.583.04.7盐酸溴代克伦特罗5085.279.680.075.882.280.63.577.768.271.182.278.975.65.850073.080.079.478.685.579.34.5溴布特罗5065.172.266.670.168.268.42.867.167.668.175.670.469.83.550072.370.870.580.176.874.14.2班布特罗5084.885.395.790.188.688.94.484.088.491.192.891.35.950081.581.988.295.492.187.86.2盐酸苯氧丙酚胺5066.966.971.285.575.673.27.878.076.073.880.585.578.84.550098.498.189.585.290.192.35.8莱克多巴胺69.568.371.176.678.272.74.42066.269.573.575.681.173.25.769.872.374.980.278.875.24.3羟甲基克伦特罗5069.876.868.975.271.172.33.572.883.581.375.580.078.64.450097.394.688.685.693.46.3盐酸克伦潘特5066.567.768.572.675.870.23.966.678.374.174.969.972.84.650089.490.881.082.674.683.76.6马布特罗5071.165.870.082.278.873.66.768.179.680.985.572.577.36.950073.872.578.680.188.678.76.4盐酸马喷特罗5070.672.973.477.280.274.83.876.676.975.786.480.779.24.450088.987.481.779.990.285.64.6缩饲料和精料补充料添加回收率,平均回收率在6化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5098.696.799.697.295.596.97.150090.395.392.694.695.593.72.2特布他林5095.293.37.096.894.193.698.55.750097.294.396.695.294.195.5沙丁胺醇95.299.596.198.93.22098.697.592.595.597.23.596.797.993.392.490.494.1齐帕特罗5096.299.293.294.196.93.588.892.392.597.694.650088.187.795.190.692.790.8西马特罗5095.297.392.297.94.692.394.190.596.697.294.12.850095.395.592.294.391.193.7西布特罗5098.896.492.799.098.492.394.497.84.450099.895.795.497.292.596.12.7利托君5094.698.392.294.394.094.72.296.293.494.196.696.33.050095.297.798.293.398.14.9克伦塞罗5095.45.098.995.493.699.95.750099.794.391.798.294.695.73.2克伦普罗5096.696.498.299.84.198.596.497.094.492.695.82.350090.891.292.194.598.293.4氯丙那林5099.195.598.295.193.396.22.486.297.487.792.894.691.74.750098.896.587.095.894.694.54.5妥布特罗5096.798.094.796.697.52.598.794.294.299.05.350094.195.992.294.398.695.02.4盐酸克伦特罗89.894.995.694.695.82084.094.288.194.695.291.24.992.684.796.498.692.192.95.3盐酸溴代克伦特罗5095.795.290.497.86.498.296.33.350093.491.090.893.495.792.92.0溴布特罗5096.692.293.697.699.494.796.694.297.23.050092.295.492.496.64.7班布特罗5093.992.394.796.795.63.285.680.380.288.687.984.54.150094.386.095.393.291.192.03.7盐酸苯氧丙酚胺5093.496.193.197.34.588.395.993.894.394.94.950096.991.994.692.495.43.8莱克多巴胺96.891.199.45.72092.895.694.298.15.693.799.992.294.793.894.93.0羟甲基克伦特罗5097.695.296.594.797.63.897.192.291.892.892.793.32.250097.795.799.32.6盐酸克伦潘特5094.990.597.698.497.35.492.890.895.997.695.194.42.750094.796.993.591.694.494.2马布特罗5093.795.098.899.65.598.02.350095.697.798.699.33.0盐酸马喷特罗5093.495.75.798.393.695.496.598.25.450090.487.989.995.694.191.63.2化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5086.990.591.189.693.390.32.390.587.890.196.090.791.03.050095.288.980.592.595.590.56.2特布他林5081.388.585.497.494.589.46.680.474.481.484.690.182.25.850081.484.282.092.588.685.74.7沙丁胺醇94.292.885.292.795.492.14.02090.893.189.896.894.95.889.275.178.895.584.684.6齐帕特罗5091.590.786.494.693.15.986.681.378.686.895.985.86.750082.882.383.292.688.885.94.5西马特罗5095.695.691.387.094.15.384.285.796.298.893.37.850077.299.884.792.185.787.98.5西布特罗5088.694.988.688.693.894.793.55.550088.486.075.795.892.187.67.6利托君5091.094.897.699.26.993.995.591.497.35.650096.786.894.899.495.85.6克伦塞罗5082.289.994.393.096.191.15.585.886.390.795.487.689.24.050086.894.893.487.590.290.53.5克伦普罗5087.884.890.995.488.585.592.093.096.091.04.150092.187.290.084.392.689.23.5氯丙那林5074.993.194.993.089.289.085.883.484.398.299.090.17.850094.090.597.488.281.690.46.0妥布特罗5081.892.791.292.489.689.54.571.385.478.689.279.480.86.950083.098.178.886.492.287.77.6盐酸克伦特罗95.699.693.583.876.189.79.62078.684.987.292.688.586.45.288.384.888.496.280.187.65.9盐酸溴代克伦特罗5087.591.286.594.07.894.684.589.996.893.46.450083.788.791.290.294.989.74.1溴布特罗5091.191.396.391.794.993.02.486.582.384.986.994.787.14.650097.499.590.386.785.291.86.4班布特罗5090.482.478.194.193.787.77.194.979.185.989.590.187.95.950097.593.789.284.593.46.9盐酸苯氧丙酚胺5083.486.981.793.489.27.887.180.682.097.792.087.97.150079.291.673.592.288.485.08.3莱克多巴胺86.584.286.289.489.36.42086.176.686.179.293.284.26.577.894.988.384.690.887.36.5羟甲基克伦特罗5089.188.595.495.897.393.24.190.878.683.893.396.588.67.350087.289.987.095.282.188.34.8盐酸克伦潘特5090.493.995.589.891.892.32.480.778.373.188.492.182.57.750082.585.682.690.284.985.1马布特罗5089.791.686.299.993.56.392.588.773.784.699.787.89.750087.899.289.279.290.289.17.1盐酸马喷特罗5087.894.484.299.893.991.492.582.089.798.090.75.850097.090.188.990.795.292.43.5化合物添加浓度回收率(%)平均回收率(%)RSD(n=5,%)卡布特罗5074.576.872.884.575.276.84.675.879.284.380.271.278.14.950095.592.091.081.190.089.95.4特布他林5087.393.885.396.594.291.44.883.889.199.094.392.291.75.750096.393.888.294.595.55.9沙丁胺醇87.287.182.195.592.888.95.32090.384.788.580.295.587.85.883.790.282.388.292.087.34.2齐帕特罗5082.582.493.391.584.586.85.284.583.690.188.295.288.34.750092.093.088.894.293.64.1西马特罗5090.699.892.286.894.87.285.296.287.586.994.590.14.950092.388.485.392.084.588.53.6西布特罗5096.286.297.592.290.092.44.696.594.291.198.06.050088.285.996.591.194.691.24.4利托君5099.491.295.589.296.294.34.198.596.592.297.397.64.050093.788.291.794.596.692.93.2克伦塞罗5087.576.090.092.588.286.86.473.574.175.084.588.279.16.850083.683.186.487.596.387.45.3克伦普罗5096.389.299.06.486.388.892.590.184.388.43.250091.599.286.382.591.290.16.3氯丙那林5083.489.184.192.180.285.84.878.686.082.792.188.985.75.250087.780.989.790.584.286.64.0妥布特罗5084.989.581.486.892.587.04.392.682.591.680.294.588.36.550093.894.984.586.881.188.25.9盐酸克伦特罗92.286.391.696.592.491.83.62081.182.574.392.487.583.66.875.287.683.585.687.683.95.2盐酸溴代克伦特罗5089.290.399.492.594.55.494.696.885.592.194.77.050077.785.577.594.589.584.97.4溴布特罗5091.386.477.496.584.587.27.286.582.183.094.692.887.85.750086.673.880.779.588.881.96.0班布特罗5093.293.690.592.182.590.44.692.297.388.485.592.291.14.450095.389.488.483.490.189.34.2盐酸苯氧丙酚胺5086.295.393.682.684.588.45.779.582.797.388.691.287.97.050088.895.290.495.96.7莱克多巴胺79.480.473.776.584.879.04.22073.689.179.087.582.182

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