1、中华人民共和国出入境检验检疫行业标准SN/T 1976-2007 进出口水果和蔬菜中畸茵醋残留量检测方法气相色谱法Determination of azoxystrobin residues in fruit and vegetable for import and export-GC method 2007-08-06发布2008-03-01实施必需主主二、:卢恕童问:中华人民共和国发布飞士?国家质量监督检验检茂总局S/T 1976-2007 前言本标准附录A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。本标准起草单位中华人民共和国青海出入境检验检疫局，甘肃农业大学食品科学与工
2、程学院，中华人民共和国辽宁出入境检验检疫局。本标准主要起草人:薄海波、孙洁、毕阳、李连通、王宏伟。本标准系首次发布的出入境检验检疫行业标准。I 1 范固进出口水果和蔬菜中畸茵醋残留量检测方法气相色谱法本标准规定了水果和蔬菜中暗茵酣残留量的气相色i告测定方法。SN/T 1976-2007 本标准适用于苹果、葡萄、柑楠、甘蓝、番茄、马铃薯、西兰花中暗茵醋残留量的测定。2 方法提要试样用乙殷乙酣十环己炕0+1)混合溶剂提取，用配有氮磷检测器的气相色谱仪测定，外标法定量。3 试剂和材料除另有规定外，所用试剂均为分析纯，有机溶剂使用前重蒸倪。3. 1 丙酬。3.2 环己烧。3.3 乙酸乙醋。3.4 氯化
3、俐。3.5 元水硫酸的。用前在650C灼烧4h.置于干燥器中备用。3.6 略菌醋标准品:纯度大于或等于99%。3. 7 标准储备溶液g准确称取适量的暗院院标准品(精确到0.1mg).用丙阴配制成浓度为1mg/mL 标准储备溶液。该溶液在18C冰箱中保存。3.8 标准工作溶液g根据需要再用环己烧+乙酸乙醋o十1)稀释成适用浓度的标准工作溶液，该溶液在0C4C冰箱中保存。4 仪器和设备4. 1 气相色谱仪，配有氮磷检测器.4.2 组织捣!i机=转速不低于20000 r/min. 4.3 旋转蒸发仪。4.4 离心机2毅大转速5000 r/min. 4.5 鸡心瓶，100mL. 4.6 具塞离心11，
4、80mL。5 试样制备与保存5. 1 试样制备取代表性样品约500g.将其可食用部分(不可用水洗)切碎后，用捣碎机将样品加工成浆状，混匀，装入洁净容器，密封，标明标记。5.2 试样保存将试样于0C4 C保存。在抽样及制样的操作过程中，应防止样品受到污染或发生残留物含量的SN/T 1976-2007 变化。6 测定步骤6. 1 提取称取20g(精确至0.01g)试样于80mL具塞离心管中，加入40mL环己炕+乙酸乙酣溶液。十1).在15000 r/min匀浆1min，加入5g氯化纳(3.4)再匀浆提取1min，在3000r/min离心5min，吸取出上清液，用2g无水硫酸纳(3.5)脱水，分取2
5、0mL于鸡心瓶中，经50C水浴旋转蒸发近干，然后用氮气流吹干。用环己炕+乙酸乙醋。十1)溶解，定容至1.0 mL.供气相色i普分析。6.2 测定6.2. 1 气相色i昔分析条件8 a) b) d) e) 1) g) h) 空气:60mL/min; i) 进样方式z元分流进样.1.5 式中-X 试样中晴雨自由残留量，单位为毫克每千克(mg/kg); A 样液中暗商醋的色谱峰面积，As 标准溶液中暗菌醋的也i苦峰面积$C一一标准溶液中p!菌醋的浓度，单位为微克每毫升(flg/mLl, V一一样液.I终定容体积，单位为毫升(mL)，m 最终样液所代表的样品质量，单位为克(g)。9 测定低限和回收率9
6、. 1 测定低限本方法的测定低限为:0.01mg/险。2 SN/T 1976-2007 添加浓度及回收率本方法添加浓度及回收率见表L表19.2 本方法添加浓度及回收率样品名称添加浓度范围/(mg/kg)回收率范罔/%苹果0.011.0 86.6-97.3 葡萄0.01- 1. 0 86.8-104.2 柑桶0.011.0 86.6-104.4 甘蓝0.01- 1. 0 85.8-105.9 番茄0.01-1. 0 81. 2-95. 2 马铃薯0.011.0 84.4-96.6 西兰花0.01- 1. 0 79.2-102.6 j / / / 3 飞飞比1412114矿iftlJJf/jyf/
7、 / /1ljj/ / / 附录(资料性附录)曙茵茵标准品的气相色i昔图A SN/T 1976-2007 MPDIB pA 130 N-VLF- 120 110 100 90 mm 12 10 8 畸茵商标准晶的气相色i昔图6 图A.14 2 80 0 4 SN/T 1976-2007 Foreword The annex A of this standard is an informative annex. This standard was proposed by and is under the charge of Certification and Accreditation admi
8、nistra tion of the Peoples Republic of China. This standard was drafted by Qinghai Entry-Exit Inspection and Quarantine Bureau of the Peoples Re public of China , Gansu Agricultural University, and Liaoning Entry-Exit Inspection and Quarantine Bu reau of the Peoples Republic of China. The main draft
9、ers of this standard are Bo Haibo, Sun Jie, Bi Yang , Li Liantong and Wang Hongwei. This standard is a professional standard for entry-exit inspection and quarantine promulgated for the first time 5 S:-.I/T 1976-2007 Determination of azoxystrobin residues in fruit and vegetable for import and export
10、-GC method 1 Scope This standard specifies the method for the determination of azoxystrobin residues in fruit and vege table by gas chromatography (GC ;三片This standard is a口plicableto the dtteimination .of azoxystrobin resifues in apple. citrus fruit. 叫乞一飞，. _ -_ f grape. cabbage. tomato. cauliflowe
11、r nd potat口fI2 Principle of determination / ./ 乒/ Azoxystrobin residue in the t臼tsam别e伊德extractedw而eth训acet剖e-cyclohexane(1 + 1 ). The 二/，i:.L/臼extract is determined by means of Gqrwith NiP detettTt1S刑铲幌temalstandard method. 3 Reagents and materials V飞芷一中j Unless other specified. all reagents were o
12、f可alytical-r3. 1 Acetone. 3.2 Cyclohexane. 3.3 Ethyl acetate. 3.4 3.5 3.6 Azoxystrobin standard , Purity:;-99 %. j J ,epf in a削ccator3.7 Stock standard solution, Accurately weigh (accurate to O. 000 1 g) azoxystrobin standard (3.邸.dissolvewith acetone to 1 mg!mL. The solution should be stored at -1S
13、oC. 3.8 Working standard solution, According to the concentration required. dilute stock standard so lution (3.7) with ethyl acetate-cyclohexane (1 +门.The solution should be stored at ot -4C. 4 Apparatus and equipment 4.1 Gas chromatography, Equipped with nitrogen!phosphorous detector. 6 SN/T 1976一2
14、0074.2 Homogenizer, The max rotate speed is 20 000 r/min 4.3 Rotary vacuum evaporator. 4.4 Centrifuge, the max rotate speed is 5 000 r/min. 4.5 Heart-shaped flask, 100 mL 4.6 Centrifuge tube, 80 mL. 5. 2 Storage of test sample The test sample should be stored at恒立兰旦旦旦analysis，6 Procedure 1 000L ethy
15、l acetate-cyclohexane (1 + 1) for analysis. 6.2 Determination 6.2. 1 GC conditions a) Column, HP-5臼pillarycolumn. 30 m X O. 25 mm( id) X O. 25m. or the equivalent, b) Column temperature, 180C for 2 min, ramp at 30t /min to 280t , hold for 10 min, c) Injection port temperature, 290t , 7 SN/T 1976-200
16、7 d) Detector temperature, 300(; , e) Carrier gas, Nitrogen purity;?o99. 999% , 1.8 mL!min. f) Trail blow, Nitrogen,purity;?o99. 999% .20 mL/min, g) Hydrogen: purity ;?o 99. 999%.4.0 mL/min. (0 -1.5) min after analysis starting hydrogen is turn off, h) Air: 60 mL!min, i) Injection mode: Splitless. p
17、urge after 1.5 min, j) Injection volume, 1.0L 6. 2. 2 Determination According to the approximate concentrat旧nof azoxystrobin residues in sample. select the working standard solution with similar responses to that口fsample solution. The responses of azoxystrobin in the working standard and the sample
18、solution should be within the linear range of the instrument. The standard working solution and the sample solution should be injected alternatively. Under the a bove gas chromatographic operating conditions. the retention time of azoxystrobin is 6. 74 min. Chromatogram of standard is shown as figur
19、e A. 1 in Annex A 7 81ank test The operation of the blank test is the same as the described in the method of determination. but with the omission of sample addition. 8 Calculation and expression of result Calculation the content of azoxystrobin residues in test sample with chromatographic data proce
20、ssor or with the formula(门.the blank value should be subtracted from the result of calculation. X = A: c. V -As.m ) 1 ( . . . . . . . . . . . . . . . . . . . . . . . . . . . . where X-the residue of azoxystrobin in test sample , mg!kg, A -the peak area of azoxystrobin of the sample solution, 8 SN/T
21、1976-2007 As-the peak area of azoxystrobin of the standard solution; c-the concentration of azoxystrobin in standard solution.g/mL; V-the final volume of the sample solution. mL; m-the corresponding mass of test sample in the final solution. 9 9 Limit of determination and recovery 9. 1 Li mit of det
22、ermination The limit of determination of this method is O. 01 mg/kg. 9. 2 Fortified concentration and recovery The fortified concentration and recovery of this method are shown in table 1. Table 1一Thefortified concentration and recovery of this method Sample Fortified concentrationl (町咱/kglRe，ye时1%a
23、pple 0.01-1.0 86.6-97.3 grape 0.01-1.0 86.8-104.2 cit阳sfruit 0.01-1.0 86.6-104.4 cabbage 0.01-1.0 85.8-105.9 tomato 0.01-1.0 81.2-95.2 potato 0.01-1.0 84.4-96.6 cauliflower 0.01-1.0 79.2-102.6 9 S:I/T 1976-2007 Annex A ( informative) Chromatogram of azoxystrobin standard MPDIB pA 盯12 NMVLF- 10 / 130 80 0 120 110 100 90 10 中华人民共和国出入境检验检疫行业标准迸出口水果和蔬菜中暗茵茵残留量检测方法气相色谱法SN/T 1976-2007 提中肉标准出版社出版北京复兴门外三里河北街16号邮政编码;100045 网址电话，6852394668517548 中国标准出版社秦皇岛印刷厂印刷晤开本880X 1230 1月6印张1字数17千字2007年11月第一版2007年11月第一次印刷印数1-20003陪书号:155066 .18257 定价10.00元
