1、共和本东SN/1017.7-2014 代替SNjT1017.7一2002出涕、电、电、电、电医呈望星墨J脱脱削弱国窍比二飞均每臼nhDetermination of aldicar险，caI如yl,oxamyl , bendioca旷band piri阻icarbresidues in cereals for export 2014-04皿09发布2014-11呻01实施中华人民共和曾发布国家庭竞量监督检雄检查变单SN月1017.7-2014目号吕SN/T 1017共分为9个部分:一一-SN/T1017.1 出口粮谷中环庚草酸残留量检验方法;SN/T 1017.2 出口粮谷中丁按磷残留量检验方
2、法;SN/T 1017.3 出口粮谷和蔬菜中戊菌隆残留量检验方法;一一SN/T1017.4 出口粮谷及油菜抨中贴菌清残留量检验方法;一-SN/T1017.5 出口粮谷及油将中快杀碑残留量检验方法;一-SN/T1017.6 出口粮谷中叶枯歌残留量检验方法;SN/T 1017.7 出口粮谷中涕灭戚、甲茶戚、杀线戚、恶虫戚、抗蜘威残留量的测定;SN/T 1017.8 进出口粮谷中哗虫琳残留量检验方法液相色谱法;一一-SN/T1017.9 进出口粮谷中毗氟乙草灵残留量检验方法。本部分为SN/T1017的第7部分。本部分是按照GB/T1.1-2009给出的规则起草。2挥部分代替SN/T1017.7-20
3、02(出口粮谷中涕灭戚、西维因、杀线戚、恶虫戚、抗蜘威残留量的检验方法。本部分与SN/T1017.7-2002相比，主要技术变化如下:一一本部分增加了玉米、小麦、大豆检验样品基质;一一一气相色谱法更改为液相色谱法、液相色谱-质谱/质谱法，降低了方法的检出限;删除了抽样部分;优化了前处理方法。请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别这些专利的责任。本部分由国家认证认可监督管理委员会提出并归口。本部分起草单位:中华人民共和国河北出入境检验检疫局。本部分主要起草人:马育松、郭春海、王敬、贾海涛、刘宝圣、邸窟。I 1 范围出口粮谷中涕灭戚、甲蔡戚、杀续戚、恶虫戚、抗螃威残留量的测
4、定SN/T 1017的本部分规定了出口根谷中涕灭戚、谱-质谱/质谱和液相SN/T 1017.7-2014 、恶虫戚、抗蜘威五种氨基甲酸自旨类农药残留量的测定。2 规范性引用文件GB/T 6682 3 原理试样中氨基甲酸醋类农药用柱或凝胶渗透色谱净化后，4 试剂和材料除非另有规定外，4.1 乙睛:残留级。4.2 甲醇:残留级。4.3 环己烧z残留级。4.4 乙酸乙醋:残留级。4.5 甲苯。4.6 甲酸:高效液相色谱级。用石墨化炭黑/氨基因相萃取4.7 氧化铀:140 oc烘烽4h，在干燥器内冷却至室温，贮于密封瓶中备用。4.8 元水硫酸铀:650 oc灼烧4h，在干燥器内冷却至室温，贮于密封瓶中
5、备用。4.9 乙腊-甲苯(3十1，体积比):量取60mL乙睛(4.1)和20mL甲苯(4.5)，混匀。4.10 环己烧乙酸乙醋。+1，体积比):将1000mL的环己烧(4.3)与1000mL乙酸乙醋(4.4)混匀。4.11 0.2%甲酸水溶液:量取2.0mL甲酸(4.的，用水定容至1000mL。4.12 定容液:取80mL 0.2%甲酸(4.11)，加入20mL乙腊(4.1)，混匀。4.13 标准物质:涕灭威(分子式:C7日14N202S , CAS编号:116-06-3)、甲茶威(分子式:C12 H10 N02 , SN/1017.7-2014 CAS编号:63-25-2)、杀线威(分子式:
6、C7H13N303S , CAS编号:23135-22皿0)、恶虫威(分子式:Cl1日13N04，CAS编号:22781-23-3)、抗蜻威(分子式:Cl1 H18 N4 O2, CAS编号:23103-98町2)，纯度大于等于99%，冷藏于冰箱中避光保存。4.14 标准储备液:精确称取适量标准物质(4.13)，用甲醇(4.2)配制成10g/mL的标准储备液，储备液在一18oC以下贮存于棕色瓶中。4.15 标准中间液:取适量标准储备液(4.14)用甲醇(4.2)配制成浓度为1g/mL的标准中间液，现用现配。4.16 基质标准工作溶液:提据需要，用空白基质溶液稀释标准中间溶液(4.1日成适合浓度
7、的基质标准工作溶滚，现用现配。4.17 石墨化炭黑/氨基因相萃取柱:500mg/500 mg/6 mL，或相当者。4.18 微孔滤膜:0.22m，有机系。5 仪器和设备5.1 液相色谱-质谱/质谱仪:配电喷雾离子源(ESI)和四极杆质量分析器。5.2 凝殷渗透色谱仪。5.3 分析天平:感量为0.01g和0.1mg。5.4 组织捣碎机。5.5 离心机，转速不小于4000 r/min。5.6 均质器，转速不小于15000 r/min。5.7 涡旋混合器。5.8 旋转蒸发仪。5.9 氮吹仪。5.10 固相萃取装置。5.11 聚丙烯具塞离心管，15mL和50mL。5.12 鸡心瓶，120mLo 6 样
8、品制备和保存6.1 制样要求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。6.2 试样的制备粮谷样品经粉碎机粉碎，混匀，分成两份，分别装入洁净容器内，一份作为试样供检栅用，另一份作为留样保存并做好标识。7 测定步骤7.1 提职称取试样约5g(精确到0.01g)于50mL离心管中，加10mL水润湿样品，30min后加入5g氯化铀(4.7)、20mL乙腊(4.1)，15000 r/min均质提取1min, 4 000 r/min离心10min，将上清液经装有10 g无水硫酸铀(4.8)的漏斗过滤至120mL鸡心瓶中。再用10mL乙睛重复以上提取过程，合并提取SN/1017.7-20
9、14 被于同一鸡心瓶中，于450C水浴浓缩至近干，待净化。7.2 净化7.2.1 大米、玉米和小麦用2mL乙腊-甲苯(4.9)榕解7.1步骤中所获得的浓缩液。用10mL乙睛-甲苯(4.9)预淋洗石墨化炭黑/氨基固相萃取柱(4.17)，弃去全部流出液。将样品提取液通过固相萃取柱，再用10mL乙腊甲苯(4.9)溶液分三次洗脱，控制流速为0.5mL/min，收集全部流出液，于45oC氮气吹干。用1.0mL乙睛-0.2%甲酸水溶液(4.12)溶解，过0.22m有机相微孔滤膜后，供液相色谱-质谱/质谱测定。7.2.2 大豆7.2.2.1 凝胶潘透色谱仪参考条件凝胶渗透色谱仪参考条件如下:a) 色谱柱:冯
10、S白X3Bio-Beads填料，粒度3招8m7陌5m，30Om丑lmX2白5mm(内径)，或丰柜自当者;b流动相:环己:烧皖-乙酸乙醋(4.10)，流速:5.0m丑lL/minc) 进样量:5mlL ; d) 净化程序:0min8 min弃去洗脱液，8min20 min收集洗脱液。7.2.2.2 凝胶潘透色谱净化程序用10mL环己烧-乙酸乙醋(4.10)溶解7.1步骤中所获得的浓缩滚，按7.2.2.1条件净化。净化后将收集的洗脱液于450C7.)(浴旋转蒸干，用0.50mL乙精-0.2%甲酸水溶液(4.12)溶解，过0.22m有机相微孔滤膜后，供液相色谱白质谱/质谱栅定。8 液相色i普-质谱/
11、质i普测定8.1 溜相色i普参考条件液相色谱参考条件如下:a) 色谱柱:C18, 150 mmX2.1 mm(内径)，填料粒度51m，或相当者;b) 柱温:30oC; c) 进样量:5L;d) 流动相组成及梯度洗脱条件见表1。表1流动相及梯皮洗膜条件时间/min流速/CmL/min)0.2%甲酸水溶液/%乙腊/%0.0 0.5 90 10 4.0 0.5 60 40 6.0 0.5 15 85 8.0 0.5 15 85 8.1 0.5 90 10 12.0 0.5 90 10 3 SN/T 1017.7-2014 8.2 质i普参考条件质谱参考条件如下za) 离子源:电喷雾离子源;b) 扫描
12、方式:正离子扫描;c) 检测方式:多反应监测(MRM);d) 使用前应调节各参数使质谱灵敏度达到检测要求，参考条件参见附录A中的表A.l。8.3 定性测定选择1个以上母离子、2个以上子离子，在相同试验条件下，样品中待测物质的保留时间与基质标准溶液的保留时间偏差在士2.5%我接草场边:雨雨如度与浓度接近的基质标准工作洛液中对应的定性离子的相对丰模毁费要在传到过如魏京的拙，则可判定为样品中存在对应的待测物。在上述仪器条件下，5相对离子丰度/%允许的相对误差/%8.4 定量测定为横坐标绘制标准工作曲线，用畸测定的线性范围内。9 空白试验除不称取样品外，10 结果计算采用外标法定量，按式(1)计算试样
13、中氨基甲酸醋类农药的含量。4 式中:X , = A , X c, X V X 000 -A;s X m , 1 000 X; 试样中农药i残留量，单位为微克每千克(g/kg);A; 试样中涕灭威等5种氨基甲酸醋类农药的峰面积;c; 标准工作液中农药t的浓度，单位为微克每毫升(g/mL); V一一样液最终定容体积，单位为毫升(mL); A;s -标准工作液中农药i的峰面积;m一一试样溶液所代表的质量，单位为克(g); 计算结果应扣除空白值。(10 士50、基质校准榕液浓度图参见附录B中的图B.L. ( 1 ) SN月1017.7-201411 mo定低限本方法对5种氨基甲酸醋类农药的测定低限均为
14、5g/埠。12 回收率范围5种氨基甲酸醋类农药在大米、玉米、小麦和大豆基质中不同添加水平的添加回收率范围参见附录C中的表C.l。13 原理14 试剂与材料除非另有规定外，所有试剂均14.1 珊砂。14.2 邻苯二甲M(O-phthaladehyde，OPA)。14.3 琉基乙醇(优级纯)。14.4 氢氧化锅。14.5 定容液z取85mL甲薛(4.14.6 混合标准工作液t根据需准工作溶液。混合标准工14.7.1 0.05 mol/L氢氧化铀溶14.7.2 0.05 mol/L础砂缓冲液t热溶解，冷却，加水至刻度，轻轻混采用石墨化炭黑/氨基固相萃取5)配制成适当浓度的混合标水，过0.22m滤膜。
15、，加入500mL水，600C水浴加14.7.3 OPA衍生试剂:称取50mg oP7f溶于少量甲醇(4劫后转入500mL容量瓶中，加入0.25mL 疏基乙薛(14.3)，加入跚砂缓冲液(14.7.2)至刻度，混匀后过0.22m滤膜。现用现配。14.8 其他同第4章。15 仪器设备15.1 液相色谱仪，配有高压梯度泵、柱后衍生反应装置和荧光检测器。15.2 其他同第5章。16 样晶制备和保存同第6章。5 SN/T 1017.7-2014 17 测定步骤17.1 提取同7.1017.2 净化17.2.1 大米、玉米和小麦净化步骤同7.2.1。用1.0mL甲醇水溶液(14.5)溶解浓缩液，过0.22
16、m有机相微孔滤膜后，供液相色谱测定。17.2.2 大豆净化步骤同7.2.2。用0.50mL甲醇水溶液(14.5)溶解浓缩液，过0.22m有机相微孔滤膜后，供液相色谱测定。18 高效液相色谱法测定18.1 液相色谱参考条件液相色谱参考条件如下:a) 色谱柱:C18柱，150mmX4.6 mm(内径)，填料粒度5m，或相当者;b) 荧光检测器:激发波长ex339nm，发射波长em465nm; c) 进样量:50L;d) 柱温:35oC; e) 流动相组成及梯度洗脱条件:见表3。表3流动相组成及梯度洗脱条件日才|同/min流速/CmL/min)甲醇/%0.0 0.8 15 2.0 0.8 15 32
17、.0 0.8 70 32.1 0.8 100 35.0 0.8 100 36.0 0.8 15 45.0 0.8 15 18.2 柱后衍生参考条件18.2.1 0.05 mol/L氢氧化铀溶液(14.7.1)，流速0.3mL/min; 18.2.2 OPA衍生试剂(14.7.3)，流速0.3mL/min; 18.2.3 反应器温度:7120-50 土2510-20 土30主二10土5050 8.4 Quantitative analsis Under the best conditions of the apparatus , inject series of matrix standard
18、working solutions sepa-ratel. The matrix standard working tration of standards.Use the curve t 气功12rsponsesversus the concen自wn sample. The responses of Id be within the linear range of the standard 9 Blank test can be found in Annex B. 丁heoperation of the blank test is th the omission of sample add
19、ition. d of determination, but with 10 Calculation an expression or according to For-Calculation the content of fumagil mula (1) 飞/a1,. /，、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . Where , X; -the residue content of fumagillin in test sample，附/kg;A; -the peak area of fumagillin in th
20、e sample solution; C; -the concentration of fumagillin in the standard working solution，崎/mL;V -the final volume of the sample solution,mL; A;s-the peak area of fumagillin in the standard working solution; 20 m -the corresponding mass of test sample in the final solution , g. The blank value shall b
21、e subtracted from the result of calculation. 11 Limit of determination The limit of quantification is 5崎/kg.12 Recovery Part 2 High 13 Principle The residues in the test sample are extracted with cleaned up with SPE cartidge of liquid chromatographwith a 14 Reagents and materials Unless specifically
22、 noted,all reagents 14.1 Borax. 14.2 O-Phthaladehyde (OPA). 14.3 Thiofluor, guaranteed grade. 14.4 Sodium hydrate. SN/T 1017.7-2014 method r concentrated , the solution is residues are then detected by detection and quant卜is redistilled water. 14.5 Dissolved solution: transfer 15 mL water into 85 mL
23、 methanol (4.2) , mix adequately. 14.6 Matrix standard working solution: According to the requirement , dilute middle standard solution (4.14) to appropriate concentration with dissolved solution (14.5). 21 SN/1017.7-2014 14.7 Post-column reagent preparation 14.7.1 0.05 mol/L sodium hydrate solution
24、: weigh 1 9 sodium hydrate(14.4) and dissolve in 500 mL wat町，andthen the solution is passed through 0.22m filter. 14.7.2 0.05 mol/L borax solution:weigh 19.1 9 borax(14.1) and dissolve with 500 mL water into a 1 000 mL volumetric flask with a bath temperature below 60 oC , cold and then dilute with
25、water to 1 000 mL. 14.7.3 OPA reagent: Dissolve 50 mg of OPA in approximately 5 mL of methanol(4.2) into a 500 mL volumetric flask,add 0.25 mL thiofluor(14.3) into the reservoir,and add the borax solution (14.7.2) to 500 mL,and then the solution is passed through 0.22m filter. 14.8 The other apparat
26、uses are the same as Section 4. 15 Apparatus and equipment 15.1 Liquid chromatography, equipped with a post-column derivative sstem and fluorescence de tection. 15.2 The other apparatuses are the same as Section 5. 16 Preparation and storage of test sample This section is the same as Section 6. 17 P
27、rocedure 17.1 Extraction 了hissection is the same as Section 7.1. 17.2 Cleaning.心P17.2.1 The sample of rice,corn and wheat 丁hecleaning-up steps are the same as Section 7.2.1. Residues are dissolved with 1.0 mL dissolved so lution (14.5). Then the solution is passed through 0.22m filter and readfor an
28、alsis. 22 SN/T 1017.7-2014 17.2.2 The sample of sobean The cleaning-up steps are the same as Section 7.2.2.Residues are dissolved with 0.50 mL dissolved solution (14.5).Then the solution is passed through 0.22m filter and readfor analysis. 18 Determination 18.1 HPLC operating conditions HPLC operati
29、ng conditions are as following: a) Column:C,s150 mmx4.6 mm (i.d.)，5m particle size or equivalent; b) Fluorescence detector:ex =339 nm，em = 465 nm; c) Injection volume:50L; d) Column temperature:30 oC; e) Mobile phases and gradient elution conditions are listed in Table 3. Table 3 Mobile phase and gr
30、adient elution condition Time Flow rate Methanol Water 内llnmL/min % % 0.0 0.8 15 85 2.0 0.8 15 85 32.0 0.8 70 30 32.1 0.8 100 。35.0 0.8 100 。36.0 0.8 15 85 45.0 0.8 15 85 18.2 Post-column conditions 18.2.1 0.05 mol/L sodium hydrate solution (14.7.1) ,0.3 mL/min. 18.2.2 OPA post-column reagent (14.7.
31、韵，0.3mL/min. 23 SN/T 1017.7-2014 18.2.3 Reactor temperature: Hydrolysis temperature: 80 oC ; derivatization temperature: room tem perature. 18.3 HPLC analysis Under the above operating condition, the standard working solution should be randomly injected in between the injections of the sample soluti
32、on of equal volume. The respond of the analte is Y-axis, concentration of standard working solution is X-axis,protract standard working curve.Quantity with standard working curve,the responses of the sample solution should be within the linear range of the instrument detection.Under the yl,bendiocar
33、b and pirimicarb is 1 chromatogram of the standard 19 Blank test The operation of the blank test the omission of sample addition. 20 Calculation an expression of result Calculation the content of mula (2). Where: X; -the residue content of fumagillin in test sample，崎/kg;A;一thepeak area of fumagillin
34、 in the sample solution; of aldicarb, carbaryl , oxam and 26.4 min , respectively. The of determination, but with processor or according to For-.( 2 ) C; -the concentration of fumagillin in the standard working solution ,ng/mL; A ;s-the peak area of fumagillin in the standard working solution; V -th
35、e final volume of the sample solution ,mL; m -the corresponding mass of test sample in the final solution , g. 24 SN/T 1017.7-2014 The blank value shall be subtracted from the result of calculation. 21 Limit of determination The limit of quantification is 10g/kg. 22 Recovery 丁heranges of recovery in
36、 diffe 25 SN/T 1017.7-2014 Annex A ( Informative) Reference mass conditions1) Reference mass conditions are as follows: a) Nebulizer:45 psiC1 psi = 6.895 kPa); b) Gas Flow:5 L/min; c) Sheath Gas Flow: 10 L/min; d) Sheath Gas emp:350 oC; e) Capillartempreture:350 oC; f) Capillarvoltage in ESI + mode:
37、 3 500 V; g) Collision gas:Nitrogen; h) Other mass operating conditions are list in Table A. 1. Table A.1 The s臼nsegment, ion pairs and collision energy of the analtes Declustering Retention time lon pairs Dwell time Compound 罚1m(m/z) potential 町1SV 208.1/89.1 20 Aldicarb 6.83 60 208.1/116.0骨20 202.
38、1/127.0 20 Carbaryl 7.62 70 202.1/145.0份20 242.0/72.1棒20 Oxamyl 4.31 150 242.0/121.0 20 223.9/108.9 20 8endiocarb 7.48 80 223.9/166.9篝20 239.3/72.1 * 20 Pirimicarb 4.86 108 239.3/182.1 20 Collision energy eV 1 10 2 30 4 10 3 10 9 21 曾markis the quantification ion pair. for the different MS equipment
39、 , the parameters may be different, and the MS parameters should be optimiazed to the best before analysis. 1) Non-commercial statement: the reference mass parameters in Annex A are accomplished by Agilent 6460 LC MS/MS, the equipment and its type involved in the standard method is only for referenc
40、e and not related to any commercial aim ,and the analysts are encouraged to use equipment of different corporation or different typ母.26 SN/T 1017.7-2014 Annex B ( Informative) MRM chromatogram of standard X104 +ESI MR岛1(239.3-72.1)2 ill 72. 1) 111 1. 4 1. 2 1 0.8 0.6 =-的目。岛的时Tme/mn XI04 +ESI MRM(239
41、. 3-182.1) 。1.5 ill 口。 口305 Tmejmn XI01 +ESI;仅M(242.0-121. 0) 6111 5.5 =-C白白。民的时5 6.5 6 5.5 4.5 5 Tmejmn 4 b) pirimi臼rbXI03 I+ESI;仅M(208.1-89. 1) 1 2 Timejmin X103 +ESIMRM(208.1-116.0) 5111 皇4 3 口8. 2 p: 1 3.5 3 2 吉1.5出 1 J 0.5 6 5.5 5 4 4.5 Tmejmin a) oxamyl X102 +ESI;仅M(223.9-108. 9) 百叫I11 8. 11 1
42、1 E叫!川Tme/min X102 +ESI MRM(223. 9-166. 9) g 8il 11 611 11 8. 411川 21111 4.5 3.5 3 9 8.5 8 7 7.5 Timejmn 6.5 6 9 8.5 8 6.5 7 7.5 Tmejmin aldicarb d) 6 5 5.5 bendio臼rblL 川口叫咱lllllll|llllllllLF一+H训川训门引HU-OOOOA丛zn，m口-EgzagMc) XI02 +ESI MRM(202. 1-127.0) 111 号311 11 21 8. 11 1才|27 7.5 8 Tmejmin e)臼rbary
43、lFigure 8.1 the MRM chromatogram of standards at 25 Jg/L 9 8.5 7 6.5 SN/1017.7-2014 Compound Bendiocarb Carbaryl Pirimicarb Oxamyl Aldicarb 28 Fortified level g/kg 5 10 20 5 10 20 5000 5 10 20 1000 5 10 20 5 10 20 Annex C (Infor阳ative)Recovery ranges Table C.1 Revery ranges Range of recovery Soybean
44、 78.6.96.0 79.6.100 82.7.97.0 78.2.98.4 80.1.97.4 80.0.100 87.8.99.6 79.9.96.2 80.0.85.9 82.0.95.0 80.0.96.0 76.6.96.1 71.0.91.2 80.1.95.2 76.5.98.3 72.1.91.4 80.5.94.9 16.00 14.00 12.00 10.00 D 且J-。20。8.00 E吕EUqd J L 3 6.OO 4.00 2.00 0.00 L 0.00 Instruction: 1一一一Oxamyl;2一一-Aldicarb;3一一Carbaryl;4一一-
45、Bendiocarb;5-一-Pirimicarb.SN/1017.7-2014 Annex D ( Informative) HPLC chromatogram of standard 4 5.00 10.00 35. 00 40. 00 45. 00 Figure D.1 50g/L 29 SN/T 1017.7-2014 Fortified level Compound g/kg 10 8endiocarb 20 40 10 20 Carbaryl 40 5000 10 20 Pirimicarb 40 1 000 10 Oxamyl 20 40 10 Aldicarb 20 40 30
46、 Annex E ( Informative) Recovery ranges Table E.1 Recovery ranges Range of recovery % Rice Corn Wheat 82.6-97.3 79.0-95.2 75.7-94.4 83.0-100 79.9-100 78.8-94.8 80.2-100 75.2-95.2 75.2-94.6 81.5-95.9 80.3-93.。74.2-90.1 78.6-100 79.3-102 80.6-96.1 84.1-101 75.6-88.1 77.7-97.2 88.2-100 91.6-100 80.0-96
47、.4 77.6-89.0 80.0-93.0 75.9-92.8 78.9-90.6 85.0-102 83.3-95.1 84.5-100 84.1-101 83.6-100 81.0-99.0 83.0-98.0 85.0-92.。78.2-94.5 79.8-90.1 75.4-90.3 89.1-101 85.4-92.1 79.8-91.9 80.1-100 74.8-97.3 82.5-96.。76.3-92.5 79.5-93.6 77.8-88.8 85.0-98.5 87.8-97.7 80.4-95.9 89.9-98.5 77.2-96.3 82.3-100 Soybea
48、n 79.2-96.0 79.2-94.8 81.3-99.0 77.8-93.。75.8-90.7 77.7-94.3 82.0-98.。75.9-101 82.1-100 78.1-95.6 80.0-95.0 71.1-92.3 80.4-95.7 82.3-94.6 74.8-91.1 80.0-91.8 78.7-91.5 立ONlh.h5FFHZ的中华人民共和国出入境检验检疫行业标准出口粮谷中涕灭戚、甲茶戚、杀线威、恶虫戚、抗螃戚残留量的测定SN/T 1017.7-2014 4延中国标准出版社出版北京市朝阳区和平里西街甲2号(100029)北京市西城区三里河北街16号(100045)总编室:(010)68533533网盘上中国标准出版社秦皇岛印刷厂印刷安开本880X 1230 1/16 印张2.25字数56千字2014年12月第一版2014年12月第一次印刷印数1-1300 定价33.00元;(. 书号:155066 2-27673 SN/T 1017.7-2014
