SN T 1985-2007 进出口动物源性食品中吩噻嗪类药物残留量检测方法 液相色谱-质谱 质谱法.pdf

1、5 中华人民共和国出入境检验检疫行业标准SN/T 1985-2007 进出口动物源性食品中盼嘻嗦类药物残留量检测方法液相色谱-质谱/质谱法Determination of phenothiazines residues in foodstuffs ()f animal origin for import and export-LC-MS/MS Method 2007-08-06发布2008-03-01实施4贯主苦头如叫出中华-JF民共和片国发布忖彗EYE国家股坐llEYiT检验检班总局中华人民共和国出人堤检验检疫行业标准进出口动物源性食品中盼唾睫类药物残留量检测方法液相色i昔-质i曹/质谱法S

2、J /T 1985-2007 * 中国标准出版社出版北京复兴门外三里河北街16号邮政编码，1000.(5网址WW电话，6852396685175,8 中国标准出版社秦皇岛印刷厂印刷峰开丰880X1230 1/16 印张1.25 字数33千字2007年11月第一版2007年11月第一次印刷fn数1.-2000 书号，155066. 218270 定价12元SiI/T 1985-2007 前言本标准的附录A和附录B均为资料性附录。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2中华人民共和回深圳出入境检验检疫局、中网检验检疫科学研究院、中华人民共和固辽宁出入境检验检疫局。本标准主要起

3、草人岳振峰、l丽琪、JJt少冰、赵凤娟、彭涛、华红慧、lD;品阳、王宏伟、侯乐锡。本标准系首次发布的出入境检验检疫行业标准。1 范国进出口动物源性食品中盼嘻瞟类药物残留量检测方法液中目色谱-质i昔/质谱法SNjT 1985-2007 本标括i规定了动物源性食品中甲苯瞅瞅、异丙昧、氯丙陈、乙阶丙、丙酷丙嗦等五种吩略嗦类药物残臼量的制样、浪仙也i昔质l昔/质i古测;1:拍l确证方法。本标准远川于肌肉、内脏、水产品和牛奶等动物源性食品中fp末路嗦、异I坷睹豆、氯丙哝、乙M丙嗦、丙Itt丙嗦等五利I吩略嗦类药物残留的J如C 2 规范性引用文件I 1 下列文il巾的条款通过本标准萨阿rmTii风及严京有

4、?海的条款可凡是i日期的引用文件，其随后所有的修改单(不包知助识的内容)或修订版均不远月1安保标准，然而，鼓励根据本标准达成协议的各方研究是否可使用这哩文件的111新版本。凡是不llJl期的引用:50 20-50 10-20 10 :1: 20 :i: 25 士30土50v x-m 内-xx-w x-4 A一X ( 1 ) 式中-X一一样品中待测组分的含量.单位为毫克每千克(mg/kg); Ax 一-l!1定液中待测组分的峰面积$As 标准液中待测组旁的呢宵节了?m-J终样液所代表的样品质髦，单位)，J觅(g) Cs 标准液中待测组乡的合茧.1(仅为毫克每升(mg/L); V一一定容体和、.单

5、位为E至于十市u.一一叩/ / 礁，即下内嚼亏l王丙嗦、乙酌ll峡、l:丙嗦均为9 泪定低限与回收率9. 1 测定低限肌肉/肾脏/肝脏/牛奶0.001 mg/kg; 鱼肉:甲苯喔9.2 回收率回收?在见表3。俨/ 可收率/%药物名称添加浓度叫k如肉叫立| 1古肝牛奶鱼肉。.O!(鱼肉为O.。1) 75vd98. l叩-10头山:-99. 5 70.0-105 60.2-98.5 甲苯哩嚓0.02C鱼肉为0.02) h5-9, -97.0 n.5-110 67.0-9;:). 。0.04C鱼肉为0.0气吗争.0I .8-1哎. 4) 亨3例-94.3 71. 8-100 71. 5-97.:;

6、0.001 71.可3-10G I口77 3-109 67.3-102 61. 8-99. 5 异丙嗦0.002 13.-0-1号3j745 号?yt5l09 73. 5-10) 65. O_9). 5 0.004 飞。-:o;vj8口cfLF / 95.0.110 77.5-109 76.5-101 0.001 65.7-102 69.7-91. 7 66.1-97.8 62.1-%.5 61. 3.96. 5 氯丙嗦0.002 H.O-98.0 I 70.5-99.0 73.0-101 69.0- 93.5 70.0- 98.5 0.004 75.0-102 70.5-99.0 77.0-

7、95.5 6-!. s-吕8.36). O- !J !l , 8 0.001 77.2-105 65.8-102 70.2-108 70. O-I(l) 62. -90.5 乙It丙嗦0.002 75.5-105 8-L5-II0 87.0-107 6!).5-105 66.5-叫O0.004 75.5-103 83.3-110 75.3-105 68. :i -!)4. j 7.t. o-n.;) 0.001 72.1-110 63.8-89.7 66.1-99. ;) 66.9-川.1 6 1. 8-9-L 5 丙耽丙嗦0.002 83.5-104 61. 0-92. 5 71. 0-99

8、. 0 65.5-川。70.0-97.5 0.004 72.8-105 75.3-97, 3 76.8-101 7:3.0-93.8 70.3-92.0 唾雪平苟安电目4 附录A(资料性附录)参考质谱条件参考质i世条件:a) 雾化气(NEBl:7.00L/min(氮气hb) 气帘气(CUR):9. 00 L/min(氮气): c) 喷雾屯压(S):2500 V; d)去i1iJ11Jiful度(TEM):500.C: e) 去i在开IJ气流7.00L/阳H1) 碰报气(CADl:6.00g) 其他Nn肯参数见表A, . 和巳伽吩哩礁类药物的主要参考质谱参数_-SN/T 1985-2007 1

9、14 器帜盲树叶咐叫化合物母同于士刘JYJ八IA-l (m/z) 甲辈暗暗/100 E唰节贸36 221.2 异丙嗦50 28:.0 50 氯内嗦31!L 1 乙Il:l丙略:!Z7. I 丙院丙睬31 1. 4 , I P 170 170 150 150 150 150 180 180 210 CEj CXP eV 39 39 12 31 14 33 18 61 4 29 6 65 10 31 8 71 4 27 6 1)非商业性声明:附录A所列参考质谱条件是在/P13000型液质联用仪上完成的.此处列出试验用仪器型号仅为提供杏考.，1不涉及商业目的.鼓励标准使用者尝试不同厂家或型号的仪器。

10、p d SN/T 1985一2007附录(资料性附录标准昂的多反应监测(MRl1)色i曹图B 22 1. 2/163. 8 10 Jl 12 13 14 15 9 285.0/197.8 88 nn 7阳7htt ) 2 i( 686 嘎UAEAA68 且;?1 10 11 12 13 14 15-= 221.2/89.8 4 3 2 9 ZSU飞、-rhu-z-5 1 4 1 3 1 2 1 1 1 0 1 285.0/85.9 ) l ( 2 9i5 4 678 Ilmin 1 5 6 7 8 rlmin -40 0 00 2 EOhFits-50 Permitted tolerances

11、 % 土508: 2 Calculation and expression 0 formula( 1) ) 1 ( . . . . . . where X the residue content of phenothiazine in the test sample. mg kg , A x Peak area of phenothiazine in the sample solution, As Peak area of phenothiazine in the standard working solution, m the corresponding mass of test sampl

12、e in the final sample solution. g , Cs the concentration of phenothiazine in the standard working solution. mg L, V the final volume of sample solution. mL. 13 SN/T 1985-2007 9 Li mit of quantifi臼tionand recovery 9. 1 Limit of quantification For the muscle, kidney , liver and milk , the limit of qua

13、ntification for xylazine is O. 01 mg/kg, and for promethazine, chloropromazine. acepromazine and propionylpromazine is 0.001 mg/kg respective. Iy, for fish muscle, the limit of quantification for all phenothiazines residues is O. 001 mg !kg 9. 2 Recovery Recovery see table 3. Table 3-Recoveries of p

14、henothiazines residues Recoveries % Compound Spiked level/(mg Ikg) Swine Swine Swine Fish Milk muscle kidney liver muscle 0.01 (Ior lish 70.8-98.2 70.2-102 70.9-99.5 70.0-105 6口2-98.5muscle 0.001 ) O. 02(lor lish xylazine 71.5-99.9 72.5-104 muscle O. 002) 80.0-97.0 73.5-110 67.0-95.0 O. 04(1or lish

15、71.0-93.0 70.8-102 73.5-94.3 71.8-100 71.5-97.5 muscle O. 004) 0.001 71. 3-106 83.5-11口77.3-109 67.3-102 61.8-99.5 promethazne 0.002 73.0-105 74.5-107 90.5-109 73.5-109 65.0-99.5 。00479.0-103 87.5-108 95.0-110 77.5-109 76.5-104 0.001 65.7-102 I 69.7-91.7 66.1-97.8 62.1-96.5 61.3-96.5 chloropromazine

16、 0.002 74.0-98.0 70.5-99.0 73.0-101 69.0-93.5 70.0-98.5 0.004 75.0-102 70.5-99.0 77.0-95.5 64.5-88.3 69.0-99.8 口00177.2-105 65.8-102 70.2-108 70.0-109 62.1-90.5 acepromaz Ine 。.0日275.5-105 84.5-110 87.0-107 69.5-105 66.5-96.0 0.0口475.5-103 83.3-110 75.3-105 68.5-94.5 74.0-98.5 0.001 63.8-89.7 66.1-9

17、9.5 66.9-93.4 61.8-94.5 propionylpromazine 0.002 83.5-104 61.0-92.5 71.0-99.0 65.5-99.0 70.0-97.5 0.004 75.3-97.3 76.8-101 73.0-93.8 70.3-92.0 u Annex A ( Informative) Reference mass conditions Reference mass conditions, a) Nebulizer gas, 7.00 Umin(Nitrogen) , b) curtain gas, 9.00 L/min(NitrogenJ ,

18、c) ion spray voltage, 2 500 V , d) heat temperature, 500t , e) heat gas, 7.口。L/min(Nitrogen); f) collision gas, 6.00 mL!min (NitrogenJ. g) Other mass operating conditions are listed in table A. 1. Table A. 1-Main MS parameters of phenothiazines Precursor Daught川nI Dwell time/ ! Compound DP FP (阿)/Z)

19、m/z)盯1S89.88 100 36 170 xyzaline 221.2 163.8 100 36 170 85.9 50 41 150 promethazine 285.0 197.8 50 41 150 58.0 50 36 150 ch!oropromazine 319.1 85.8 50 36 150 58. O 50 51 180 acepro盯，azlne327.1 85.8 50 51 180 58. l 50 51 210 341.4 85.9 50 51 210 SN/T 1985-2007 CE! CXP eV 39 4 39 12 31 14 33 18 61 4 2

20、9 6 65 10 31 B 71 4 27 6 Note:For the different MS equipment.the parameters may be different.and the MS parameters should be optimized to the best before analysis. a H旧rkis the quantification ion. 1) Non-commercial statement: the reference mass parameters in Annex A are accomplished by API 3 000 LC-

21、MS/MS. the equipment and its type involved in the standard methoQ is only for reference and not related to any commercial aim. and the analsts are encouraged to use equipments of different corporation or different type 川/11985-2007 Annex B C Informative) Multiple reaction monitoringCMRM)chromatogram

22、 of standard solution 二IOOe1 0.001 10 11 12 1:3 14 15二i 40 e 00 2 ru、二三-zu-FL-22 1. 2/163. B 10 11 12 13 14 15 9 285.0/197.8 6 7 8 I/ l11 in 5iR 5 6 7 8 tlmin 22 1. 2/89. 8 四14且54 3 2 9 678 I/mtn 5. H (2) 4 3 2 f U 飞, z p u 10 11 12 13 14 15 E: 285.0/85.9 删丘之主-JEU-z。10 1I 12 13 14 15 9 4 3 2 9 678 f

23、hnin 5 4 3 2 319.1/85.8 500 。坷，民o 飞, J 寻ZJ亘o 11 12 13 14 15三319.1/58.0 5.69 (盯。oo o riJ，-?PJ-z 10 11 12 13 14 15 9 4 3 2 9 678 111m 5 4 3 2 327, 1/85.8 JO 11 12 13 14 15 9 311.4/85.9 ) 4 ( 9 2 5 6 7 8 IJm ll1 5.53 (5) L 5 6 7 8 I/min 酬。r-u飞h-zzu四Z-5 4 2 0 327.1/58.0 5. .30 (.1) 日创。JhJ，-FJFFUMg 5 4 3

24、 2 9 6 7 8 !/min 5.53 (5) 日4 3 2 5。, 巳飞，飞, 三 o II 12 t:J 14 15二3-1 1. 1(58. I m F一之二ZF卫王。10 11 12 la 14 15 9 Xyzallne.O.02唱L，Promethazine.O.002 mg L; Chloropromazine.O.002口咱L，Acepromazine.O.002 mg L: propionylpromazine.O. 002 mg L Figure B. l-Multiple reaction monitoring(MRM)chromatogram of 5 phenothiazines residues of standard working solution 4 3 2 9 678 Ifr日日4 3 2 (1 ) (2) (3) (4) (5) 书号:155066.2-1827012 , 00 7巳定价g