SN T 1924-2007 进出口动物源食品中克伦特罗、莱克多巴安、沙丁胺醇、特布他林残留量的检测方法 液相色谱-质谱 质谱法.pdf

《SN T 1924-2007 进出口动物源食品中克伦特罗、莱克多巴安、沙丁胺醇、特布他林残留量的检测方法 液相色谱-质谱 质谱法.pdf》由会员分享，可在线阅读，更多相关《SN T 1924-2007 进出口动物源食品中克伦特罗、莱克多巴安、沙丁胺醇、特布他林残留量的检测方法 液相色谱-质谱 质谱法.pdf（21页珍藏版）》请在麦多课文档分享上搜索。

1、 中华人民共和国出入境检验检疫行业标准SN/T 1924-2007 进出口动物源食品中克伦特罗、莱克多巴肢、沙丁肢醇、特布他林残留量的检测方法液相色谱-质谱/质谱法Determination of clenbuterol , ractopamine , salbutamol and terbutalin residues in foodstuffs of animal origin for import and export-HPLC 2007-05-23发布2007-12-01实施中华人民共和国发布国家质量监督检验检度总局 SN/T 1924-2007 目IJ1=1 本标准的附录A和附录B为

2、资料性附录。本标准由国家认证认可监督管理委员会提出并归口。本标准起草单位:中华人民共和国上海出入境检验检疫局、中华人民共和国河南出入境检验检疫局、中华人民共和国湖南出入境检验检疫局、中华人民共和国江苏出入境检验检疫局。本标准主要起草人:邓晓军、朱坚、郭德华、李波、杨冀州、戴华、陈惠兰、郭俊峰、王美玲、陈墨莲。本标准系首次发布的出入境检验检疫行业标准。 1 范围进出口动物源食品中克伦特罗、莱克多巴胶、沙丁肢醇、特布他林残留量的检测方法液相色谱-质谱/质谱法SN/T 1924-2007 本标准规定了动物源性食品中克伦特罗、莱克多巴胶、沙丁肢醇、特布他林残留量的制样和测定方法。本标准适用于动物源性食

3、品肌肉和内脏中克伦特罗、莱克多巳胶、沙丁肢醇、特布他林残留量的检测。2 试样制备与保存2.1 试样制备从所取全部样品中取出有代表性样品约500g，充分绞碎，混匀，均分成两份，分别装入洁净容器内。密封作为试样，标明标记。在制样的操作过程中，应防止样品受到污染或发生残留物含量的变化。2.2 试样保存将试样于一180C保存。3 方法提要试样中的药物残留采用pH5.2的乙酸镀缓冲、溶液提取，同时加入盐酸葡萄糖醒试酶芳基硫醋酶进行酶解后，提取液经Cl8和SCX双SPE柱净化，液相色谱质谱进行测定，内标法定量。4 试剂和材料除非另有规定，均使用分析纯试剂，水为超纯水。4.1 甲醇:液相色谱级。4.2 乙睛

4、:液相色谱级。4.3 乙酸钱。4.4 乙酸乙醋。4.5 氢氧化钱。4.6 盐酸。4. 7 甲酸。4.8 冰乙酸。4.9盐酸葡萄糖醒试酶芳基硫酸醋酶:含盐酸葡萄糖醒试酶134600 U/mL，芳基硫酸醋酶5200 U/mL 4.10 乙酸锻缓冲溶液:0.02mol/L，pH二5.2。溶解1.54 g乙酸锻于900mL水中，用冰乙酸调节pH到5.2士0.1，最后用水稀释到1L，于十40C贮存，使用期为1个月。4.11 乙酸乙醋氢氧化锻(97十3，体积比)。使用前搅拌，同时用超声波水浴超声便成均相。4.12 盐酸溶液:0.03mol/L。取30mL, l mol/L的盐酸溶液用水稀释到1Lo 4.1

5、3 标准品:特布他林(分子式:Cl2 HI9)J(丸，CAS号:23031-25-6)、克伦特罗(分子式:Cl2 Hl8 C12 N2 0 CAS号:37148-27-9)、队克伦特罗、沙丁肢醇(分子式:C , H21 NO, CAS号:18559-94-9)、战沙丁肢醇、 SN/T 1924-2007 莱克多巳胶(分子式C18H2l JO, CAS号:97825-25-7)、D莱克多巳胶纯度二三98%。4.14 标准储备液的配制(1.0 mg/mL) :分别称取约50mg ( :l: O. 1 mg)的特布他林、莱克多巴胶、克伦特罗、沙丁肢醇标准品于50mL容量瓶中，用少量甲醇溶解，然后用甲

6、醇配成1.0 mg/mL标准储备溶液。低于50C保存，有效期为1年。4.15 同位素内标标准储备液的配制(1.0 mg/mL):分别称取约50mg(士o.1 mg)的n)克伦特罗、抗沙丁肢醇、队莱克多巴胶标准品于50mL容量瓶中，用少量甲醇溶解，然后用甲醇配成1.0 mg/mL 标准储备溶液。低于50C保存，有效期为1年。4.16 1.昆合标准中间、溶液的配置:用甲醇分别稀释标准储备液至终浓度约为1.0g/mL和100.0 ng/ mL，低于50C保存，有效期为6个月。4.17 1.昆合同位素内标标准中间榕液的配置:用甲醇分别稀释同位素内标标准储备液至终浓度约为100. 0吨/mL，低于50C

7、保存，有效期为6个月。4.18 标准工作液的配置:根据需要，临用时吸取一定量的混合标准中间溶液(4.16)和混合同位素内标中间标准溶液(4.17)，用水稀释配制成适当浓度的混合标准工作溶液(参考线性浓度范围为0.5ng/mL 10 ng/mL) ，每毫升该混合标准工作溶液含有同位素内标各1.0吨。低于50C保存，有效期为6个月。4.19 Cl8 SPE柱:LC-18Sep Pak 500 mg , 3 mL或相当者。4.20 SCX SPE柱:LC-SCX Sep Pak 500 mg , 3 mL或相当者。4.21 水相滤膜:0.45mo5 仪器和设备5.1 液相色谱串联质谱仪:配有电喷雾(

8、ESl)离子源。5.2 涡旋混合器。5.3 离心机:转速二三4000 r/mi口。5.4 旋转蒸发器。5.5 感量天平(0.1mg和0.01g)。5.6 超声波发生器。5. 7 恒温箱。5.8 真空过柱装置。5.9 吹氮浓缩装置。5.10 粉碎机。6 测定步骤6.1 提取称取10g(精确至o.1 g)试样，于50mL塑料离心管中，加入20mL pH为5.2的乙酸锻缓冲溶液(4.10) ，在2000 r/min下涡旋泪合2mino添加200.0L同位素内标物(4.17)于待测样品中。加50L的卢盐酸葡萄糖醒试酶芳基硫醋酶，加盖后超声提取15mi口。在恒温箱中于370C酶解16h。以3 800 r

9、/min离心10min后，将上清液过0.45m滤膜(4.21)取5mL滤液于10mL带刻度的玻璃试管。6.2 净化将C18小柱(4.19)和SCX(4.20)小柱按从上到下的次序装好。依次用5mL水、5mL甲醇和5mL 0.03 mol/L盐酸(4.12)、溶液以1.0 mL/min的流速过柱活化。转移过滤后的提取液至固相层析柱的顶部，以0.5mL/min流速过固相层析柱，此步操作至少需要10mi口。用5mL水、5mL甲醇淋洗小柱，在较强的负压下抽10mino取下Cl8小柱。用12mL 1昆合均匀的乙酸乙醋氢氧化镜、溶液(4.11)，洗脱SCX柱子上的待分析成分并收集洗脱液，并在吹氮浓缩装置上

10、于400C士50C的温度下蒸干。加入 SN/T 1924-2007 1. 0 mL乙睛十水(l十9)振荡、溶解残渣后过o.45m滤膜。滤液供液相色谱质谱测定。6.3 测定6.3. 1 高效液中目色谱条件a) 色谱柱:C18柱，150mm(柱长)X2. 1 mm(内径)，粒度5m;b) 流动相:A:乙睛十0.1%甲酸，B:2mmol/L乙酸锻水榕液十0.1%甲酸;流速:200L/min，梯度洗脱程序见表L表1梯度洗脱程序表流动相比例/c%)梯度时间/min流动相A流动相B。10 90 3 严50 50 7 50 50 8 10 90 12 10 90 c) 柱温:35C;d) 进样量:30L，6

11、.3.2 质谱条件a) 离子源:电喷雾ESI，正离子;b) 扫描方式:多反应监测MRM;c) 雾化气压力(GSl)、气帘气压力(CU町、辅助气流速(GS2)均为高纯氮气或其他合适气体;使用前应调节各气体流量以及离子源温度(TEM)使质谱灵敏度达到检测要求，详细条件参考附录A;d) 电喷雾电压(lS)、碰撞电压(CE)、去簇电压(DP)、碰撞室入口电压(EP)、碰撞室出口电压(CXP)应优化至最佳灵敏度，监测离子对和定量离子等详细条件参考附录A，6.3.3 定量测定根据试样中被测物的药物含量，选取响应值相近的标准工作液(4.18)同时进行分析。标准工作液和待测液中四种药物的响应值均应在仪器线性响

12、应范围内。如果含量超过标准曲线范围，应用乙腊+水(l十9)稀释到合适浓度后分析。在上述色谱条件下的待测药物的参考保留时间分别为3.0min(沙丁肢醇)、3.1min(特布它林)、9.4min(莱克多巴胶)和9.9min(克伦特罗)，标准溶液的选择性离子流图参见附录B，6.3.4 定性测定按照液相色谱串联质谱条件测定样品和标准工作溶液，如果检测的质量色谱峰保留时间与标准品一致，定性离子对的相对丰度，是用相对于最强离子丰度的强度百分比表示，应当与浓度相当标准工作溶液的相对丰度一致，相对丰度允许偏差不超过表2规定的范围，则可判断样品中存在对应的被测物。表2定性确证时相对离子丰度的最大允许偏差相对离子

13、丰度/c%)允许的相对偏差/c%)6.4 空白试验50 士20除不加试样外，均按上述操作步骤进行。7 结果计算和表述20至5010至20士25士30用色谱数据处理机或按式(1)计算样品中待测药物残留量。计算结果需扣除空白值。三二10士503 SN/T 1924-2007 C X Ci X A X Ai X V X二(1 ) C ,i X A, X A X m X 1 000 式中:X 样品中待测组分残留量，单位为毫克每千克(mg/kg); E 标准工作榕液中药物的浓度，单位为纳克每毫升(ng/mL); Ci 样液中内标物的浓度，单位为纳克每毫升(ng/mL); A 样液中药物的峰面积;Ai 标

14、准工作溶液中内标物的峰面积;V 样品溶液最终定容体积，单位为毫升(mL);Csi 标准工作溶液中内标物的浓度，单位为纳克每毫升(口g/mL); A, 样液中内标物的峰面积;A 标准工作溶液中药物的峰面积;m 最终样液代表的试样质量，单位为克(g)o注.待i则药物采用相对应的同位素作为内标，特布他林采用同位素标记的沙丁胶醇作为内标。8 测定低限、回收率8.1 测定低限(LOQ)本方法肉和肝的测定低限为o.000 5 mg/kg 0 8.2 回收率8.2. 1 肉中克伦特罗、莱克多巴胶、沙丁肢醇、特布他林添加浓度及回收率试验数据见表30表3肉中克伦特罗、莱克多巴股、沙丁肢醇、特布他林回收率数据表药

15、物名称添加浓度/(g/kg) 回收率范围/C%)药物名称添加浓度/(g/kg) 回收率范围/c%)0.5 73. 496. 4 0.5 80.891.6 克伦特罗1. 0 98. 5126. 5 沙丁胶醇1. 0 104. 7 110. 9 2.0 86. 5102. 0 2.0 73. 578. 5 0.5 90. 698. 8 0.5 80. 6 108.。莱克多巳胶1. 0 91.7108.9 特布他林1. 0 90.097.3 2.0 90. 698. 8 2.0 80. 6 108.。8.2.2 肝中克伦特罗、莱克多巳腊、沙丁胶醇、特布他林添加水平及回收率试验数据见表40表4肝中克伦

16、特罗、莱克多巴脏、沙丁肢醇、特布他林回收率数据表药物名称添加浓度/回收率范围/c%)药物名称添加浓度/回收率范围/C%) (g/kg) (g/kg) 0.5 94.6100.8 0.5 77. 289. 8 克伦特罗1. 0 78. 398. 4 沙丁胶醇1. 0 77. 392.。2.0 90. 599.。2.0 73. 580.。0.5 96. 4 100.4 0.5 77. 290. 6 莱克多巴胶1. 0 95.5122.0 特布他林1. 0 80.594.9 2.0 92. O108. 5 2.0 73. O79. 5 4 a) 电喷雾电压(l曰:5500V;b) 雾化气压力(泊1)

17、:50Pa; c) 气帘气压力(CUR):20Pa; d) 辅助气流速(GS2):30 Pa; 巳)离子源温度(TEM):550C; 附录Al)(资料性附录)质i普参数SN/T 1924-2007 f) 碰撞电压(CE)、去簇电压CDP)见表A.1所示。碰撞室入口电压(EP)为10V、碰撞室出口电压(CXP)为13V。表A.1p-兴奋剂及内标碰撞电E、去簇电压参数表母离子(Ql)m/z子离子(Q3)m/z碰撞电压/V去簇电压/V203.0 18 45 克伦特罗277.3 259.2 20 50 164.2 12 50 莱克多巳胶302.3 284.3 22 50 148. l 25 55 沙丁

18、胶醇240.2 222.1 17 75 152. l 23 48 特布它林226.2 107. 1 43 45 Dq克伦特罗286.3 204.0 16 75 D5莱克多巴胶307.2 167.2 15 45 川沙丁胶醇243.2 15 1. 1 22 55 a 为定量离子对。1) 附录所列参数是在All4000质谱仪完成的，此处列出试验用仪器型号仅是为了提供参考，并不涉及商业目的，鼓励标准使用者尝试不同厂家和型号的仪器。5 SN/T 1924-2007 附录(资料性附录)标准品MRM图谱B Max.2.7e4 cps 9. 36 1-9.0 10.0 11.0 XIC ot+MRM (1 3

19、 pairs) : 277.3/259.2 amu trom Sample 3 Cstd 3) ofDala061120.认itfCTurbo Spn可277/259克伦特罗2.5e41 fl- 2.0c41 ，、Ic 1. 5c41 i3 1. Oc4j -三岳000.010.0 8.0 7.0 6. 0 岳.04. 0 nu nu 。-.2.0 1. 0 Max.9. 1e4 cps 9. 36 l 9.0 10.0 XIC of+MRM (13 pairs) : 277.3/203.0 amu from Samplc 3 Cs!d 3) ofOa!a061120.川ffCTurbo Sp

20、ray) 277/203克伦特罗l11411-1l111hl-|l41-BiBilH444440 UOLUOLWOL-inununununU QUOOPOA吁向， 司、的porH-mEOHE一11. 0 MFIU川丛8.0 7.0 6. 0 岳.04. 0 nu nu 2.0 1. 0 XIC ot+MRM (1 3 pairs) : 286.3/204.0 amu trom Sample 3 Cstd 3) ofDala061120.认itfCTurbo Spn可286/204 09克伦特罗 n 1lft-ill-M匹(44440C CCCC内7000队川-l qundn41i 司、的por

21、H-mEOHE一XIC of+MRM (13 pairs) : 302.3/284.3 amu from Samplc 3 Cs!d 3) ofOa!a061120.川ffCTurbo Spray) 8.96 1 9. 0 11. 0 10.0 8.0 7.0 6. 0 岳.04. 0 nu nu 2.0 1. 0 Max.3. 1e4 cps 302/284莱克多巴胶11. 0 10.0 Max.2. 1e4 cps 1. 0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 XIC ot+MRM (1 3 pairs) : 302.3/164.2 amu trom Sample 3

22、Cstd 3) ofDala061120.认itfCTurbo Spray) 8.9岳l 9. 0 3.0c4 , 2.0c41 1. Oc41 。电 司、的porH-mEOHE一302/164莱克多巴胶 的2.0c410. , - 乒1.5e44 的22j 1. Oe41 己1一l5000.01 0.0 XIC of+MRM (1 3 pairs) : 307.2/167.2 amu from Samplc 3 Cs!d 3) ofOa!a061120.川ffCTurbo Spray) i 克仑特罗、莱克多巴肢标准品的多反应监测(MRM)图谱11. 0 10.0 8.0 7.0 6. 0 岳

23、.04. 0 nu nu 2.0 1. 0 Max.3780.0 cps 307/167 D5-莱克多巴胶11. 0 10.0 2.0 图B.11. 0 ilL川nununununuc 8000内哼tnununu口qdqdqL1EU 司、的porH-mEOHE一6 SN/T 1924-2007 Max.3. 4c4 cps XIC oC十MRM(13 pairs) : 226.2/1岳2.1 amu Crom Samplc 3 C std 3) oC Oata061120川IT(T urbo Spray) 226/152特布他林川il川丛川4J引lJ什1钊1)pwnLPwnLr飞4000队33

24、21 的巳QPCZZOHE2.0 11. 0 10.0 9. 0 8.0 7.0 6. 0 岳。Max.7840. 0 cps XIC oC十MRM(13 pairs) : 226.2/107.1 amu仕omSamplc 3 C std 3) oC Oata061120.川IT(T urbo Spray) 226/107特布他林4. 0 1. 0 llL巾。00001AUZnununurl oonununuru 7642二的且tAEEZ】巳.,. 11. 0 Max.2.0e4 cps 4严310.0 9. 0 .,. 9. 0 争8.0 240/222沙丁肢醇7.0 国XICoC十MRM(

25、13 pairs) : 240.2/222.1 amu Crom Samplc 3 Cstd 3) oCOata061120 叭1日二(T urbo Spray) 2. 79 1 1. 0 2. 0 3. 0 4. 0 5. 0 6. 0 7. 0 8. 0 XIC oC十MRM(13 pairs) : 240.2/148.1 amu Crom Samplc 3 Cstd 3) oCOata061120 叭1日二(T urbo Spray) 6. 0 岳。2.0 1. 0 2.0e4, 山，1. 5c4j . I 1. Oc4j 巳.E 5000.0j 0.0区11. 0 11. 0 Max.

26、6. 4c4 cps 10.0 10.0 240/148沙j肢醉9. 0 2. 79 | 1. 0 2. 0 3. 0 4. 0岳o6.0 7.0 8.0 回XICol十MRM(13 pairs) : 243.2/151. 1 amu仕omSamplc 3 C std 3) oC Oata061120.川IT(T urbo Spray) 6.0c4j 0. :; 4.0c4j 吉2.0e钊0.0 Max.6810.0 cps 243/1岳103- ;):1; r肢醉-r 1 I t-ill-!1i4i1MErt、nununUAUnuc inununu1 8000wu 6642U 的且tAhi-

27、【山口】巳11. 0 10.0 9. 0 自.07.0 nu nb 5. 0 4. 0 字=2.0 nu l 7 特布他林、沙丁肢醇标准品的多反应监测(MRM)固谱圄B.2 SN/T 1924-2007 Foreword Annex A and B of this standard are informative annexes. This standard was proposed byand is under the charged of certification and accreditation administa tion of the People s Republic of C

28、hina. This standard was drafted by Shanghai Entry-Exit Inspection and Ouarantine Bureau of the People s Republic of China , Henan Entry-Exit Inspection and Ouarantine Bureau of the People s Republic of China , Hunan Entry-Exit Inspection and Ouarantine Bureau of the People s Republic of China ,Jiang

29、su Entry-Exit Inspection and Ouarantine Bureau of the Peoples Republic of China. The standard was mainldrafted by Deng Xiaojun , Zhu Jian ,Guo Dehua , Li Bo , Yang Jizhou , Dai Hua , Chen Huilan ,Guo Junfeng ,Wang Meilin , Chen Molian. This standard is a professional standard for entry-exit inspecti

30、on and quarantine promulgated for the first time. Note: this English version , a translation from the Chinese text , is solelfor guidance. 8 SN/T 1924-2007 Determination of clenbuterol , ractopamine , salbutamol and terbutal in residues in foodstuffs of animal origin for import and export HPLC-MSjMS

31、 method 1 Scope The standard specifies the methods of sample prepafation and determination of clenbuterol , racto pamine , salbutamol and terbutalin residues in foodstuffs of animal origin by HPLC-MS/MS. This standard is applicable to the determination of clenbuterol , ractopamine, salbutamol and te

32、rbutalin residues in meat and viscera of animal oringin bHPLC-MS/MS. 2 Preparation and storage of test sample 2. 1 Preparation of sample The combined primary sample is reduced to 500 9 which is totally minced and divided into two equal portions, each portion is placed into a clean vessel as a test s

33、ample , which is then sealed. In the course of sampling and sample preparation , precaution should be taken to avoid contamination or any factor that may causes the change of residue content. 2. 2 storage of sample The test sample should be stored at - lSoC. 3 Principle Clenbuterol , ractopamine , s

34、albutamol and terbutalin residues are extracted from the test sample with pH5.2 ammonium acetate buffers followed by hydrolysis with glucosidase. The extract is cleaned up by SCX and C18 solid phase column. Four residues are determined by HPLC-MS/MS ,and quantified by isotope internal standard metho

35、d. 4 Reagents and materials Unless otherwise specified ,all the reagent used should be analytical grade,water is deionized water. 9 SN/T 1924-2007 4. 1 Methanol. 4.2 Acetonitrile:HPLC grade. 4.3 Ammonium acetate. 4.4 Acetic ether. 4.5 Ammonium hydroxide. 4.6 Hdrochloric acid. 4.7 Formic acid. 4.8 Ac

36、etic acid. 4.9卢-glucuronidase:100 U/mL. 4.10 Ammonium acetate buffer:O. 02 mol/L, pH = 5.2. Weigh 1.54 9 Ammonium Acetate in 900 mL wat町，adjustpH to 5.2 :t O. 1 with acetic acid and add water to final volume of 1 L. 4. 11 Acetic ether-ammonium hydroxide solution (97 + 3 , V / V). Mix to homogeneous

37、phase before use. 4.12 0.03 mol/L HCI. Dilute 30 mL 1 mol/L HCI to final volume of 1 L with water. 4.13 Clenbuterol (C12H1SC12N20 CAS:37148-27-9) , ractopamine (C1sH23N03 CAS:97825-25-7) ,salbu tamol (C13 H21 N03 CAS: 18559-94-9) and terbutalin (C12 H1S N03 ,CAS: 23031-25-6) , 0Clenbuterol， 0 ractop

38、amine , D3-Salbutamol standards: purity98%. 4. 14 Stock standard solution of clenbuterol , ractopamine, salbutamol , terbutalin (1.0 mg/mL): ac curately weigh 50 mg (士O.1 mg) standard in volumic flask, add to the bottles a known amount of water to produce a solution containing compounds all at 1.0 m

39、g/mL and store refrigerated at 50 20 to 50 10 to 20 豆豆10Permitted relative tolerances/ (%) :t 20 :t 25 :t 30 士506.4 81ank te5t The operation of the blank test is the same as the described in the method of determination, but without addition the sample. 7 Calculation and expression of result Calculat

40、ion the content of clenbuterol , ractopamine, salbutamol and terbutalin residue in the test sam ple by HPLC-MS/MS data processor or according to the formula (1). The blank value should be sub-13 SN/T 1924-2007 tracted from the above result of calculation. X = _E_ x c; x A x A 5; X V c5; X A; X A5 x

41、m x 1 000 、，FaEI /h . . . . . . . . . . . . . . . . . . . . . . . . . . . . . where X-the residue content of -agonist in the test sample,mg/kg; c-the concentration of -agonist in standard working solution , ng/mL; c;-the concentration of internal standard in sample solution ,ng/mL; A-the peak area o

42、f -agonist in sample solution; A 5;-the peak area of internal standard in standard working solution; V-the final volume of the sample solution , mL; c5;-the concentration of internal standard in standard working solution , ng/mL; A ;-the peak area of internal standard in sample solution; A5-the peak

43、 area of -agonist in standard working solution; m-mass of test sample of final sample solution ,g. (Annotation: AII卢-agonistemploy the corresponding isotope as the internal standard respectively except that terbutalin uses D3-salbutamol as the internal standard) 8 Li mit of quantitation(LOQ) and rec

44、over 8. 1 Li mit of quantification (LOQ) The limit of determination of the method for liver and meat is 0.000 5 mg/kg. 8. 2 Recovery 8.2. 1 According to the experimental data , the fortified concentration of clenbuterol , ractopamine , salbutamol and terbutalin in meat and its corresponding recovery

45、 are showed in Table 3. Table 3-Recovery阳ngeof clenbuterol , ractopamine,salbutamol and terbutalin in meat Concentration/ Recovery range/ Concentration/ Recovery range/ Chemicals Chemicals (g/kg) (%) (g/kg) (%) 0.5 73.4-96.4 0.5 80.8-91.6 Clenbuterol 1.0 98.5-126.5 Salbutamol 1.0 104.7-110.9 2.0 86.

46、5-102.。2.0 73.5-78.5 0.5 90.6-98.8 0.5 80.6-108.。Ractopamine 1.0 91.7-108.9 Terbutalin 1.0 90.0-97.3 2.0 90.6-98.8 2.0 80.6-108.。14 SN/T 1924-2007 8.2.2 According to the experimental data , the fortified concentration of clenbuterol , ractopamine , salbutamol and terbutalin in liver its correspondin

47、g recovery are showed in Table 4. Table 4-Recovery range of clenbuterol, ractopamine,salbutamol and terbutalin in liver Concentration/ Recovery range/ Concentration/ Recovery rang日/Chemicals Chemicals (g/kg) (%) (g/kg) (%) 0.5 94. 6100. 8 0.5 77. 289. 8 Clenbuterol 1.0 78. 398. 4 Salbutamol 1.0 77.

48、392.。2.0 90. 599.。2.0 73. 580.。0.5 96. 4100. 4 0.5 77. 290. 6 Ractopamine 1.0 95. 5122.。Terbutalin 1.0 80. 594. 9 2.0 92. 0108. 5 2.0 73. 079. 5 15 SN/T 1924-2007 Annex A) Cinformative annex) Main Mass Parameters a) Electrospray capillary voltage: 5 500 V; b) GS1 :50 Pa; c) CUR:20 Pa; d) GS2:30 Pa; e) lon source tempeture:550oC ; f) Ouali