【商检行业标准(SN)】 水果蔬菜中吡虫啉、吡虫清残留量的测定 高效液相色谱法

中华人民共和国出入境检验检疫行业标准SN/T 1902—2007
水果蔬菜中吡虫啉、吡虫清残留量的测定高效液相色谱法
Dcternination of imidacloprid and acctamipridresidues in fruits and vegetables-HPLC2007-05-23发布
中华人民共和国
国家质量监督检验检疫总局
2007-12-01实施
本标准的附求A为资料性附求.
本标准由区家认证认可监督管理委员会提出并力口，本标滩山中华人民共和国江苏山人境恰验检接局负市起草本标滩主要起草人；布松俞哗、7小、张爱东，刘一军、孙建洲，本标准系首次发布的检验检疫行业标准。KAONKAca-
SN/T1902—2007
一范围
水果蔬菜中吡虫嘛、吡虫清残留量的测定高效液相色谱法
本标舰定了水果蔬菜中吡以啉，吡虫清残留量的高效液相色谱测定方法，本标准适压一番茄、黄派、杜橘中此出琳、此出清残留量的验2测定方法
2.1试样制备
SN/T 1902—2007
将所取源始样品筑分出1k.取可食部分，经纠织捣碎，均分成两分.装入洁净奔器内，作为诚栏，密时,并标明标记
2.2试样保存
将试样于18℃以下冷冻保存，
：在试详制齐过程中,应防止样品受到污染或发生残留物舒丘的变化2.3方法提要
试栏中残研的吡虫林、此虫清用乙肩提取，提娘液经弗岁单矽杜净化，浓缩、楚容后，用配分紫外检测器或一极管牢列检测器的高效液相色谱仪测定。2.4试剂和材料
除为有规定外,所月试剂均为芬析纯为蒸馏水或太离了水。2.4.1乙晴：HPIC级Www.bzxZ.net
2.4.2正凹烷
2.4.3内酮，
2.4.4氯化钠：140.烘烤1h
2.4.5吡以啉标准号：纯度人于等于96为。2. 4. 6吡与清标雅品：纯度大下等于 96%。2.4.7吡出晰，吡出清标准溶液：谁硫称取适量的吡虫啉、吡出清标准品，月之腊配制成100以/11-L的单个标雅储备液.根据需要非用乙睛水（3017G)稀释成适当浓度的混介标弹工作济液2.4.8固利i萃取柱，弗婴电矽柱（Florisil)，体积3ml.小性，充物500)mg.2.5仪器设备
2.5.1高效液相谱仪：配有紫外检测器或二板管阵列检测器。2.5.2振两器。
2.5.3氮次仪。
2.5.4旋转蒸发仪。
2.5.5漩讽混个器。
2.5.6微注刻器：100l.
2.6测定步骤
2.6. 1提取
称取 25 g试样（精确牟0. 01 多),置」:250 rml 且塞催形瓶中,准确加人 50. C rmI 乙磺,放置2 h,菌提取3) rmin 后用滤纸过滤。滤液收集到装有5 名～7氯花钠的lcu ml.其塞量筒，益1子，刷SN/T 19C2—2007
烈振荡」min,在窄翌下的止［rin,使乙清相和水相分层。HTTKAONTKAca-
从19mlH塞量筒中坡取10.0 rml.乙靖溶液,移人12rml.梨形瓶中，」 i0℃水浴中旋转浓缔至近干：加人10mL丙：正已烧（10：90)溶解2.6.2净化
将弗罗里矽补用2 mI.正己烷预游洗，溶剂液面到达栏吸附层表面时,立即倒人样品辫液，充去流出液，用511内一正巴烧（1C一S0)涮洗桑形筑片淋洗弗罗甲夜柱，弃流出：用1C11L内1正已(20「3C)分芮次淋洗归罗矽相、而15mI.刻度离心管接妆洗脱液。将仁洗税凌的离心管置」氮吹仪,在\水下，氮吹至近「用乙腈十水（十70)容至2.ml.，在漩涡混含器「混约,经3.45 μrm滤膜过滤后得测2.6.3测定
2.6. 3. 1
液相色谱参考条件
色谱柱:Ds-C:5 um.250 m%4 (内希)或相当柱；色谱机湿度：40%；
流动相+Z腈水,榜度:G =nin.(595);15 rmin.(251 75):20 rmir,(5「95);d
流速:1.0 ml./min;
险测波长：258tm
f)泄样员:20 μI。
2.6.3.2色谱测定
根据样液中被测农药残留限要求·选定浓度相近的混合标准工作溶液：混合标准工作落液利得测液牛农药的含量在仪器检测的线性范圈内按1.述色谱条件逆有测定，吡业淋和吡清的架时间约为 1a nin 和 15 min。标准品的液相色谱图参见附录 A,2. 6. 4 空白试验
除不加远样外，接上述测定少骤逊行。2.7结果的计算和表达
鞍武（)语算诚栏中出啉、批出清的残留量，结果需将空门佰扣除X=A×cxV
试样吡球吡清含量，单位为毫克每千克（/k）：试样它吡虫穿，吡丧清的峰而积；标准二作液十吡小啉，吡虫清的浓度、羊位为微克每率厂（g/mI.）；样液晟终定容体积,单位为毫升(ml.)：A.
标准二作液中批出啉、吡出清的峰而积；m
最终样液所代衰的流样呆，单位为克（只）3测定低限、回收率
3.1测定低限
本方法测定低限为0.02g/kg
3.2回收率
3.2.1番中吡虫琳，吡出清的添川浓度及其收率的实验数据添加浓度在.02rg/kg时，比业啉回收率为91.4%~109%，吡清回收率为95.5108%：
添浓茂在0/g时，吡±收率为89.%101%，吡虫清叫牧率为0.※～2
102%；
SN/T1902—2007
添浓度在.[0，此虫啉收率为7~88.，此虫清收率为.103%
黄派中吡出琳批出清的添加浓度及其回收率的实验数据：系浓壹准0,02rg/kg时，此重世收率为98.5%~~105%，吡虫清回收率为91.0为~105%;
添加浓度在6.05m/kg时.批电啉回收率为95.c%-~105%，吡电清回收率为90.0%-102%；
-添加浓度在C.1c rng/kg 对，此虫嘛四收率为 81.4头~97.2，此虫清凹收率为96.2~109%。
柑概中吡虫琳、吡出消的添加浓度及具川收率的实数：3.2. 3
添浓度在c.02mg/k时，吡虫嘛叫收率为94.！%102%，吡±滑间收率为0.0～90.c乐;
添加浓度在℃,05 mg/kg 吋.吡出啉回收率为88.℃%~98.41%、此出消回收率为84.4%~93.8%
添加浓度作c.10 mg/kg时，吡业清叫收率为81.9%109%，吡出清周收率为87.3%99.5岁-
SV/T 19C2—2007
-0. 25手
附录A
（资斜性附录）
标准品高效液相色谱图
标准品液相色谱图(0.08 μg/mL.)16
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Foreword
AnnexA of this standard is an informative oneSN/T 1902—2007
This standard was praposed by and is under the charge of National Regulatory Commission for Certi-fication andAccrcditation.
This standard was drafted by Jiangsu Entry-Exit Inspection and Quarantine Bureau of the People'sRepublic of China.
The main drafters af this standard are He songtao, Yu ye, Yi Xiaojuan.Zhang aidong, Liu yijun, Surjiangang.
This standarcd is an inspection and quarantine professional standard promulgated for the first time.Nute: This English version.a trarislalior Frorn the Chinese Lext,is solely for guicanee3
S.V/T19C2—2007
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Determination of imidacloprid and acetamipridresidues infruitsandvegetablesHPLcScope
This standard specifies the method of determination of imidacloprid and acetamiprid residues infruitsandvegelablesbyHPLc.
This standard is applicable to the detcrminatian of imidacloprid residuc in tamatocs,cucumbcrs andoranges.
2 Method of determination
2. 1Preparation of test sampleThe combined primary sample is reduced to 1 kg, the edible portions are blended, and divided intotwo cqual portions. Each portion is placcd in a clean containcr as thc test sample, which is thcn scaledand labeled.
2. 2Storage of sample
The test sample should be stored below18c.Note: In the course of sample preparation, precautions must be taken to avoid cantamination or any factors that maycauso the changc of rcsicuo contont.2.3Principle
The imidacloprid and acetamiprid residues in the test sample are extracted with acetonitrile. The ex-ract is cleaned up by Flarisil sPE lube and evaporaled. The residue is dissalved and rnade up lo adefinite volume. Determination is made by mearis of a HPLC with UV detector or DAD.2. 4Reagents and materials
Unless otherwise specified, all the reagents used should be analytically pure. \ Water\ is distilledwater or de-ionized water.
2.4.1Acctonitrile:HPLCgradc
N-hexane,
2.4.3 Acetone.
2.4.4 sodium chloride:baked at 14o'c for 4 h.Imidacloprid standard:Purity no less than 96%.2.4.5
2. 4.6 Acetamiprid standard; Purity no less than 96%.SN/T1902—2007
2. 4.7 Imidacloprid and acetamiprid standard solution; Accurately weigh an appropriate amount ofimidacloprid or acelamiprid standard.dissolve in acelonitrile [o prepare a sinigle slandard stock solu-tion of 100 g/mL. Dilute the standard stock solution with acetanitrile-water (30 I 70) to the re-quired concentration as the mixed standard working solution,2.4.8SPE tube,Florisil.3 mL.500 mg.2. 5 Apparatus and equipment2. 5. 1 High performance liquid chromatograph equipped with UV detector or DAD.2. 5. 2
Shaker,
Nitrogenevaparalor.
Rotary evaporator.
Vartex mixer.
Micro-syringe:100 μL
2.6 Procedure
Extraction
Weigh 25 g (accurate to 0. a1 g) of the test sample into a 250 mL conical flask with stopper.accu-rately add 50. 0 mL acetonitrile and set aside for 2 h. Filtrate after shiaking for 30 min. Gather filtrateinlo a 100 mL measuring cylinder in which 5 g~7 g sodiurn chloride are placed. Stopper the rmeasur-ing cylinder and shake vigorously for ca 1 min,then let stand for separating completelyTransfer 10. 0 mL acetoritrile layer into a pear-shaped flask,condense it near to dryness with rotarycvaporator in a bath of 50'℃ ,dissolvc thc rcsiduc with 1α mL acctonc-n-hcxanc (10+ 90).7
S.V/T19C2—2007
2. 6. 2 Clean up
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Candition the SPE tube with 2 mL n-hexane.add the sample solution into the SPE tube when theabove solution arrive the sorbent suirface,reject the effluents, Rinse the pear-shaped flask with 5 mlacetone + N-hexane (10 + SD). reject the effluents. Then rinse the SPE tube with 5 mL acetone + N-hexane (20 + 80) and once again, collect the elution with 15 mL scale centrifugal tube. Condense nearta dryness with nitrogen evaporator in a bath o[ 50t. The residue is dissolved with 2.0 mL acetani-Irile + water (30+ 70),and mixed with the vorlex mixer, filered through a 0. 45 μrm mernbrane andready for HPLC determination.2.6.3
Determinatian
2. 6. 3. 1HPLC operating conditionColumn:ODS-C(5 jμxm).250 mm ×4 mm(i. d. ) or equivalent;a)
Column temperture:40'℃ :
c) Mabile phase : acetonitrile + water,gradient:0 min.5% ; 15 rrin,25% :20 min.5% ;d
Flow rate: 1. 0 mL/min:
e)Detector wavelength:258 nm;f) Injection volumne:20 μL.2.6.3.2HPLC determination
According to the approxirnate coricentration of the pesticide in the sarnple solutior,select the mixedstandard working solution with similar peak area to that of the sample solution, The responses ofpesticide in the mixed standard working solution and sample solution should be within the linearrangc of thc instrumcntal dctection. Under thc abovc chramatographic condition, thc retention timeof imidacloprid and acetamiprid is ca 13 min and 15 min. For HPLc chromatogram of the standard, seealso annex A.
Blank test
The operalion pf blank lesl is the sarne as hal described in lhe rrelhod of delerrmnination bul withorissior of sarrple addition.Calculation and expression of the result2.7
Calculate the content of imidacloprid or acetamiprid in the test sample according to the formula (1) .S
the blank value should be substracted from the result of calculation.×-A×c×V
SN/T1902—2007
Xthe residue content of imidacloprid or acetamiprid in the test sample.mg/kg;Athe peak area of imidacloprid or acetamiprid in the sample soluion;c the concentration of imidacloprid or acetamiprid in the stancdard working solution,g/mL;V the final volume of the sample solution,mL:Asthe peak area of imidacloprid or acetamiprid in the standard working solution;mthe corresponding rmass of the lest sarmple in the final sample solulion-g.3 Limit of determination and recovery3. 1 Limit of determination
The limit of determination of this method is 0. 02 mg/kg.3.2Recovery
3. 2. 1 Accarding to experimertal data, the fortifying cornicentrations af imidacloprid arid acetarmipridin tomato and their corresponding recoveries are:0. 02 mg/kg, thc rccovcry of imidacloprid and acctamiprid is 91. 4% ~ 109% and 95. 5% 108% :—0. 05 mg/kg , the recovery of imidacloprid and acetamiprid is 89. 2% ~ 101% and 90. 0% ~ 102% ;0, 10 mg/kg, the recovery of imidacloprid and acetamiprid is 80. 7% ~88. 5% and 85. 5% ~103%.3. 2. 2 According to experimental data, the fortifying concentrations of imidacloprid and acetamipridin cucumber and their corresponding recoveries are:0. 02 ng/kg , the recovery of irnidacloprid anid acetamiprid is 98. 5% ~ 106% and 94. 0% ~ 106% :0. 05 mg/kg , the recovery of imidacloprid and acetamiprid is 95, 0% ~ 106% and 90. 0% ~102% :0. 10 mg/kg,the recovery of imidacloprid and acetamiprid is 81.4% ~97. 2% and 96. 2% ~109%.3. 2. 3 Accarding to experimental data, the fortifying concentrations af imidacloprid and acetamipridin orange and their corresponding recoveries are:0.02 mg/kg,the recovery of imidacloprid and acetamiprid is 94.5% ~102% and 90.0% ~99. 0% ;0. 05 mg/ kg, the recovery ol imidacloprid and acetamiprid is 88. 0% ~98. 4% and 84. 4% ~93. 8% ;0. 10 rmng/kg , the recovery of irnidacloprid and acelamiprid is 84. 9% -~ 109% and 87. 3% ~99. 5% .9
SV/T 19C2—2007
-1. 25 手
Annex A
(lnformative)
HPLC chromatogram of the standardstuop.
Figure A, 1-HPLC chromatogram of the standards (0. OB μg/mL)10
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