【商检行业标准(SN)】 进出口粮谷和油籽中虫酰肼残留量的检验方法 气相色谱串联质谱法

中华人民共和国出入境检验检疫行业标准SN/T1738—2006
进出口粮谷和油籽中虫酰肼残留量的检验方法
气相色谱串联质谱法
Inspcction or lebufenozide residucs in cereals andoil seeds for import and export-Gas chromalography mass speclrometry nethod2006-01-26发布
数码防伤
中华民共和国
国家质量监督检验检疫总局
2006-08-16实施
牢标准的附录A为资料性附求
木标准由[家认计认可监督管理委员会提出并归：。本标推起学单位：中华人民儿国市私出人境检验检疫局，本标准主裳起市人：上明泰、牟、峻、邹明强声利车、游双、刘洪涛本标准系百次发布的出人境检验检行业标准，SV/T1738—2006
1范围
进出口粮谷和油籽中虫酰肼残留量的检验方法气相色谱串联质谱法
54/11738—2006
本标准是广造出！粮谷利油籽中虫酰耕残留量检验的抽样,制样和气和色质谱检测方法，本标雄川进昌…糙米，去米、大就、花生仁中止酰肼残留量的检验。2抽样和制样
2.1检验批
以不超过0:1为检验兹，20：袋装糙米约4000袋：袋装下不或大节约220装；袋装花牛的袋，来战大在时为故装品，
同检购批的商晶成以有析同特征，如包装、标记、产虑、现格和等级等、2.2抽样数量
2.2.1袋装货品
按或计算机样袋数：
全批袋数：
加样紫数
净：伯最装效小数湾分间闻世尚为整2.2.2散积货品玉米或大豆）
货准离度1超意，接货堆面积划区设点，以50m为一个取样区·册区设中心及叫作（度边m处5个点：旬增加·个样区,增设3个点2. 3抽群工具
2.3. 1全需单体收样器：全长55 cm包书于柄),直径1. 5 cr1~2. (1 cm,沟槽长度应整过袋时角线长度的
2.3.2金属效管报详器：全长分1、2m均包括手柄两部，内、外管同部位分段川儿个撕1：.个曲「 m们宽2.0cn～5，肉管的内经为5机～3. m或样器的探头长约+ tn.
2.3.3玻样铲或段样
2.3.4分样．
2.3.5带样器：窄哎袋·游封
2.3.6夺样布遇销举物
2.4抽样方法
2.4.1袋装抽样
2.4.1到也样：从雄埃的各部微髓机排最.：规的成栏效药1:年每批一股不少」3袋）将袋缝线排帮川平丁分样布或他温净的铺挚物上，效乐紧提袋底阅所·提起成用倒地药「的，必袋内贷物全活倒：李容装内程装间鼎质是各均司，鸠认情况掌后最样铲随祝自各部发排最样品并那将样品倒人熔样靠内：有装排段样品的数计声店东致SN/T 1738--2006
2.4.1.2袋内抛样：接2.2.1规定的抽样袋数（扣除倒包抽样袋数）、在雅垛四压的「：、下各层以曲线形向陷随机抽取：然后按糙米、玉米、大花：.用下述力法进行波样：对糙米，初合属单件取性器（2.3.1)槽11朝下.从每袋·角依斜对角方向拥入装内，然后将管博旋转侧上，抛出报样器，文即将样品倒人盛样器内，刘长米或大立.闭1Ⅲ长的金属双套管收详器（2.3.2），关闭槽口.从每袋角依斜对角方问拥人袋内，然后旋转出管以开片槽门，待样晶流满内管厅·再施转内管以美闭槽口，拉出取样器，立印将样品倒人样器内
对花生将应抛各袋拆开袋1缝线3计心计，用较样勺从开1处抽取样品，立印缝好袋，并将所取样品人盛样幕内：
每袋抽取样品的数量成与2..1．基本致。为挑所抽取的样品总量应不少于4kg。2.4.2散积抽样
按2.2.2规定的取择点，逐点抽取样品，籽收栏器（2.32)槽11关闭，以倾斜+5据人货墙个相应深度旋转取样器内管以天启州：，等样品流满内管后，再旋转内管以美闭槽。谢出取样器，文即将样品倒人盛样器内，从各点所拍取书品的数量成基本保持一致。做批所抽取约样品总量应不少于1k.2.4.3大样缩剑
袋装样品：合并从倒包和袋内抽样所全部样品，倒于分样布上，叫分栏板接同分法缩分样品至不少下2k-倒人整样靠内·加判后标明标记，并技时送交实验室。放码样萨：将拉反的全部样品·例于分详被「以下按上述袋装样品方法进行，2.5试样制备
2.5.1制样工具
2.5. 1.1 增作机
2.5.1.2粉筛机
2.5.1.3筛子，2.（mn圆孔烯
2.5.1.4分样板。
2.5.1.5盛祥概：其案；11．
2.5.2制样方法
2.5.2.1糙米、宝米或大更试样制备：将样品接国分法箱分全1k-用碎机（2.、。：）全部臀碎片通过20筛。混.均分成两份作为战样，分装人洁净的盛样瓶内，密闭标明标记。2.5.2.2花牛仁减栏制备：将样品按因分法统分至500名.门榜机（2.6.1.2）粉，使全部通过2.mn网孔筛。混约，均分成两份龈作为试样分装人活落的盛样瓶内，密时，标明标证2.6试样保存
将试样于～以下避光保存。在拍样及制样的操作过程小，应防止丫站受到污染或发生残物含量的变化
3测定方法
3.1方法提要
试样用水丙酮提取，提股池经二氯中炕液液分配以弗必电砖土柱净化·气相色谱-质蓝测定外标法是员。
3.2试剂和材料
除分有舰定外.所用试剂均为分析纯，水为次蒸馏水。3.2.1丙响：甩留。
3.2.2一氛甲统：蒸谱
3.2.3正已烷量燕
3.2.4乙酸乙酯：单蒸。
无水硫酸;6t.灼烧h.于密封容器中备用3.2.5
硫酸钠水溶：20岛[.c
SN/T 1738--2006
韩岁里硅十层析用.10月--200口,650℃灼烧61用前于133%清化4-冷师作加人（质3.2.7
带分数)水说活·于密划荐器中齐用3.2.8虫饼标准品，纯度99为.
3.2.9虫既肼标准溶液：准确格取适的虫酰删标雄品用少景的丙酮溶解.并以内必配制成滋度为1.，m.的标准佛各波。根据需要再用内酮稀释放活用浓度的标准1准液：3.3仪器和设备
3.3.1气州色谱质谱仪：工有质量选择检测器（MSI))。3. 3. 2娠菌。
航转热发器。
3. 3.4无水硫酸钠科:7.em1. 5 er内径）.内装5 tm高元水硫酸钠。3.3.5弗里础1补25cm1m(内降).白下而1依次填装2m高无水硫峻纳、g带数上、2Tm高无水硫酸钠，使川前用5mI上巴燃预淋洗3.4测定步
3.4.1提取
称取群约℃ 精确至.1)于25 m.上寒形瓶加人10 ml.水，放2b然陪加人[::m丙酮+振荡提最 nit!将提最液划滤丁 分波蒲斗,残淤功 m.闪谢重复提次，台并滤液下上述分液蒲斗
人20m!. 硫羧钠水溶液乱 100 r1:1氯早烷振摇3 1in,予置分,收集二象甲烷相，水相山2大试。甲重复提没两次-合并一氮甲烷。经无水硫梭钠殊脱水.改集于2I.欲缩粘中：」10水溶中旋转浓缩于证干.加人5nl二烷溶解残滑3.4.2净化
将样液倾人兆罗卫硅1杆中.依次川50ml.证己炕利50mL乙酸乙酯一止已炼（+9）进行淋洗弃共流山液：也同50 m1.乙酸z酯而己院1：1进行洗脱,收集全部洗脱液于0ml.浓缩瓶，水浴中旋转浓缩至近用内胡辫解片能容至51供知色谱-质谱测症，3.4.3测定
3.4. 3. 1气相色谱-质谱条件
色谱位：30) m×0.2mm内径）,膜厚0.25mm,1317存英细背杆：或当者台谱柱温度：50T(2 min-t 205℃(1 min)一mz 270% (7 mir):避样山温度270：
色谱质谱接|「温度,260：
载气：氧气.纯度09.399.1.2 ml.1:in:进样量：1
丑样方式：分流过样，l.min后卡阀：电离试,l：
离能鼠rV
电了含增器业压：l.kV：
测定方式送择离监浏方式：
选择监测离了(m:2):193,207,278:SN/T 1738-2006
m）溶剂延选：5nmin，
3.4.3.2气相色谱-质谱测定
根据样液被测袋药含量，选定浓度相近的标准作溶液，标准工作溶液和测样液农药的响应值均应在仪器检测的线性范压内，对标准工作溶液与样液等体积参折进样测定：在1这气相的谱质语条件下，止耕的保留时间药为了i，标准品的气相色谱谱选择离子色谱图利质谢图参见附录A图A1和录图
3.4.3.3气相色谱-质谱确证
对标准箔液及样液均按3.4.3.1规定的条件逃行測定时，姐果样液与标准溶波的选举离子疼中.在相间保留时有峰出现.则根据选择离了m/z193、207、278(其半度比8635：100)对其确证：3.4.4空白试验
除不加试样外均按上达测是步骤进行。3.5结果计算和表述
用色谱数据处理机或楼式(2算试样中出酰肼残留量：X
试样业啡残留鼠，单位为毫克句克（gkg）样液中虫酰肼的色谱峰高，单位为笔米mm)；标准T作液中虫酰肼的色谱峰高，单位为毫米（mm）；标滩作液叶业酰肼的浓度，单位为微克每毫（g/m)；V
样液最终定容休积,单位为常几(nI)：最终样效所代表的试详质民，单为克（），4测定低限、回收率
4.1测定低限
本方法的测宽低限为0.10mg/kg：4.2回收率
4.2.1糙米中业酰肝的添期浓度及其收率实验数据： 0. 10 mg/kg ~ 1. 0 mg/kg 时,间收率为 88. 2%~~95. 4% 4.2.2中虫疏的游加浓度及其率实验数据：在 0. 10 /kg~1, 00 /kg时,间收率为88. 6% --9=, 4 .4.2. 3大中出酰服的添加浓度及其向妆率实验数据：f: 0. 10 mg/kg ~ 1. 03 mg/kg 时-叫1率为 92. 7% --17. 7%.4.2.4花:1中去供的添加浓度及其收率实验数拱在.10mg/kg~1.0:ing/kg时，回收率为91.8%-~1.1%1
附录A
（资料性附录）
虫酰肼标准品的气相色请-质谱选择离子色谱图17. :78
虫酰肼标准品的气相色谱-质谱选择离子色谱图附录
：资料性附录】
虫酰肼标准物的气相色谱-质谱图27R
152165
221 235 219 235
296 911325 3341
虫酰肼标准物的气棺色谱-质谱图SN/T1738—2008
SV/T1738—2006
Foreword
AnnexAofthis standardare informativeannexThis standard was proposed by and is under the charge of the Certification and Accreditation Admin.istration of the People's Republic of China.This standard was drafted by the Jilin Entry-Exit Inspection and Quarantine Bureau of the People'sRepublic of China.
This main drafter of this standard is Warig Mingtai, Mu Jun, Zoui Mingqiang. Lu Lijun, Lu Qingshuang,Liu Hongtao
This standard is a professiornal standard promulgated for the first time.Note:This English versign.a trarislatiun from the Chinese text.is solely for guidance.6
SN/T1738--2006
Inspection of tebufenozide residues in cereals andoil seeds for import and export---Gas chromatography mass spectrometry methodScope
This standard specifies the method of sampling, sample praparation and determination of tebufeno.zide residues by gas chromatography-mass spectrometry in cereals and oil seeds for import and export.
This standard is applicable to the determination of residue content of tebufenazide in unpalishedrice, maize. soybean and peanut for import and export.2 Sampling and sample preparatian2. 1Inspection lot
Each inspection lot should not exceed 20o t. An inspection lot of 20o t. for unpolished rice in pagsshall be ca 4 000 bags: for inaize or soybean in bags shall be ca 2 200 bags; and for pearnut in bagsshall be ca 2 4oo bags. The cargo of rmaize ur soybear is su'ietimes in bulk.The characteristics of the cargo within the same inspection lot. such as packing. mark. origih, spec-ification. grade etc. . should be the same.2. 2 Quantity af sample taken2.2.1 Cargo in bags
Calculate the number of bags to be taken by formula (1))-VN
whare:免费标准bzxz.net
total nurnber of bags in a tot:number of bags to be taken.
Note: If vale a is with decirnal. round off the decinal par. which is added as unity to the integral part of a.2. 2. 2 Cargo in bulk (maize or soybean)The height of the cargo pile should not exceed 2 m. Set up areas anid spots far sampling on the pileSN/T 1738—2006
surface.50 m' is considered as an area, in which 5 spots shall be fixed. onc in the center and four atfour corners (1 m from the margins) of the area. For an additional area. thrce more sampling spotsshall be [ixec.
2. 3 Sampling topls
2.3. 1 Metallic sampler: Length(including handie): 55 cm; diameter: 1. 5 cm-2. 0 cm: groovelength: longer thain half the diagonal length of the bag.2. 3. 2 Metallic double-casing sarmpler: length 1 m. 2 m (both including handlo) with some slats ondifferent sections and respectively at the same heights for both inner and outer casings: length ofslots: 15 cm~20 cm, width of the slots: 2.0 cm~2. 5 cmt inside diameter of the inner casing:2. 5 cm~3, 0 cm: the probe length of the sampler: ca 7 cm.2.3.3Sampting shovel or Fadle2.3.4Plate for quartering.
2. 3. 5 Sarnple container: Can or bag, which can be sealed2. 3. 6 Cloth (or other suitable rmaterial) sheet: For sample dividingtquartering).2.4 Sampling pracedure
2. 4. 1For cargo in bags
2. 4. 1. 1 Surripling by emptying out : Draw 10 percent of the number of bags specified in 2. 2. 1(natless than 3 bags) at any part of the pile at random. Unseam and open the bag, and lay it on a cleancloth sheet ( or other clean sheet), Grasp tight two corners of the bag bottom and raise up to an angleof 45\. tug backward for ca 1 m until all content of the bag is emptied out. Chieck whether the qualityof goods is uniform within and between the bags. After confirming the gouds are in normal condiLion. scoop up the sample from different parts of the out-poured content at random, and promptlyplace in a sample container.The quantity of sample drawn from each bag shauld he basically thesame.
2. 4. 1, 2 Sampling from inside the bags: Draw the samples from the number of bags specified in2. 2. 1. by dedlicting the nlimber of bags drawt in 2. 4. 1. 1) as follows: Along t!ie sine wave of thepile. draw thc sanples from the bags of upper. middle and lower parts around the pile at random.For unpolishecl rice or maize proceed as follows:For unpolished rice. using the metaltic sampler(2.3. 1), insert it with its groove facing downward.ciagonaliy into each bag, then turn the sampler 180'.draw out the sampler and promptly pour thesample into a coritainer.
SN/T 1738--2006
For 1naize or soybesr. lising the metallic double-casing sampler (2. 3. 2) (the slots should pe clusedwhile inserting inidiagionally into each bag. Turn the inrer casing to open the slots so that the sampiemay fill up the inrer tube. Again turn the inner casing to c ose the slots and draw out thc sampler.Promptlypour the sanple into a sample container.For peanut. partially unsearnt3 stitches~5 stitches) the bag mouth, scoop out the sample from eachbag with a iaalciat the hag opening. Promptly close the bag by seaming, anid pour the sample into asample container.
Tie arnount of sample clrawn from cach hag should be basically the same as in 2. 4. 1. 1. The totalweighitof ihesarmpleof eachi latshouldbenot lessthan4kgSamplingfrornthecargo inbulk:2. 4. 29
Insert the double-casing sampler(2. 3. 2) successively into the pilc at the sputs specified in 2.2. 2. toappropriate doptn at 45'(the slots should be closed while nserting :n), Tirn the inner casing to openthe slots so that the sample may fill up the inner tube. Again turn the inner casing to close the slutsanid draw out the sampler. Promptly pour the sample into a sample container. The amount of sampledrawn [rom ali the spots shall be basically the same.The total weight of the sample of each lot should he not less thari 4 kg.2. 4. 3Reduction of gross sarnpleFor cargo in oags: Pour all the samples I [rorn both a) and b)l on a clean sheet. Reduce to nol lessthan 2 kg by cuartering with a plate. Place in a samiple container. seal, label and senct te the laborato.ty in time.
For cargo in buik: Pour all the drawn saingle onto a clean s:heet anci proceed as [or cargo in bags dle.scribedabove
2.5Preparation of test sample2. 5. 13
Sainpling tools
2. 5. 1. 1
Grinder
2. 5. 1. 2Pulverizer
2. 5. 1. 3 Sieve: 2. 0 mrn round-hole sieve2. 5. 1. 4 Plate for quartering.SN/T1738—2006
2.5. 1.5 Samiple container: Wide-mouth bottle. with ground stopper.2.5.2Procedure
For unpolished rice, maize or soybean: Reduce by quartering to ca 1 kg. Grind with a2. 5. 2. 1
grinderc2. 5. 1. 1) to let all pass through a 20-mesh sieve. Mix thoroughly atnid divide into two equalportions, place in clean sample containers as the test samples: seal and label.2.5.2.2For peanut: Reduce by quartering to ca 500 g. pulverize with a pulverizer(2.5.1. 2) lo letal pass through a 2. o mm round-hole sieve. Mix thoroughly and divide inta two equal portions as thetest samples, place in clean sanple containers, seal and label.2, 6 Storage of test sample
The test samples should be stored o' ~4C and kept away fram light. In the course of sampling andsample preparation. precautions must be taken to avoid cantamination or any factors that may causethe change of residue contant.3Method of determination
3. 1Principle
The test sample are extracted with water-acetone, the extract is partitioned with dichloromethaneCleaned up by passing through a on Florisil column. Determination is made by means of a Gc-Ms, u.sing external standardmethod.3. 2 Reagents andl materialsUnless otherwise specified. all the reagents used should be analytically pure. \water\ is distilled wa-ter.
AcetoneRedistilled.
3.2.2Dichloromiathane:Recistilled.3.2.3n-hexane:Redistilled.
3.2.4Ethylacetate:Redistilled.3. 2. 5 Anhydrous sodium suilfate: Igrite at 650C for 4 h,and keep in a tightly closed container.10
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