T-CTES 1037-2021 纺织用植物染料 茜草染料

ICS87.060.10CCSG57T/CTES1037—2021纺织用植物染料茜草染料Vegetabledyesfortextiles—Rubiacordifolia2021-03-16发布2021-04-15实施中国纺织工程学会发布IT/CTES1037—2021本文件按照GB/T1.1—2020《标准化工作导则第1部分：标准化文件的结构和起草规则》的规定起草。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专利的责任。本文件由中国纺织工程学会标准化技术委员会提出。本文件由中国纺织工程学会归口。本文件负责起草单位：武汉纺织大学、常州大学。本文件参加起草单位：烟台明远创意生活科技股份有限公司、广东溢达纺织有限公司、爱慕股份有限公司、淄博祥源纺织有限公司、重庆三五三三印染服装总厂有限公司、德州恒丰纺织有限公司、厦门市特步儿童用品有限公司。本文件主要起草人：姜会钰、纪俊玲、薛志勇、周立明、姚金波、李文伟、王文、周绚丽、秦晓霞、刘玉庆、李苏红、孙颖、杨宏、智军、白濛、徐鸣、王智。T/CTES1037—2021I纺织用植物染料茜草染料本文件规定了植物茜草染料的要求、采样、试验方法、检验规则以及标志、包装、运输和贮存。本文件适用于从茜草植物来源提取的植物染料。2规范性引用文件下列文件中的内容通过文中的规范性引用而构成本文件必不可少的条款。其中，注日期的引用文件，仅该日期对应的版本适用于本文件；不注日期的引用文件，其最新版本(包括所有的修改单)适用于本文件。GB/T2374—2017染料染色测定的一般条件规定GB/T2386—2014染料及染料中间体水分的测定GB/T2390染料pH值的测定GB/T3920纺织品色牢度试验耐摩擦色牢度GB/T3921—2008纺织品色牢度试验耐皂洗色牢度GB/T3922纺织品色牢度试验耐汗渍色牢度GB/T4841.1染料染色标准深度色卡1/1GB/T5713纺织品色牢度试验耐水色牢度GB/T6678—2003化工产品采样总则GB/T6682分析实验室用水规格和试验方法GB19601染料产品中23种有害芳香胺的限量及测定GB20814染料产品中重金属元素的限量及测定GB/T24101染料产品中4-氨基偶氮苯的限量及测定T/CTES1023—2020纺织用助剂生物质特性鉴别方法碳14法3术语和定义下列术语和定义适用于本文件。3.1茜草rubiacordifolia化学名称：1,2-二羟基蒽醌1,2-二羟基-9,10-蒽醌；分子式：C₁₄H8O₄相对分子量质量240.21;CAS号：72-48-0;分子结构式：2T/CTES1037—20213.2天然性naturality从茜草等含有蒽醌类衍生物的植物根茎中提取制成的染料，不含任何化工合成有机物质。4.1茜草染料的质量应符合表1的要求。表1茜草染料的质量要求有害芳香胺的质量分数/(mg/kg)重金属元素的质量分数/(mg/kg)4.2茜草染料在棉织物上的染色性能和牢度应符合表2的规定。表2茜草染料在棉织物上的染色性能和牢度耐洗耐汗渍耐摩擦耐水色牢度酸碱变色棉沾毛沾变色棉沾毛沾变色棉沾毛沾干湿2-32-32-32-32-32-33以批为单位采样，生产厂以一次拼混均匀的产品为一批。每次采样数应符合GB/T6678—2003中7.6的规定。所采样产品的包装应完好，采样时勿使外界杂质落入产品中。采样时探管采取包括上、中、下三部分的样品，所采样品质量不少于500g。将采取的样品充分混匀后，分装于两个清洁、干燥、密封良好的容器中，其上黏贴标签。注明：产品名称、批号、生产厂名称、取样日期、地点。一个供检验，一个保存备查。T/CTES1037—20213柠檬酸柠檬酸在自然光线下采用目视评定。6.2pH的测定按GB/T2390的规定进行测定。按GB/T2386—2014中3.2烘干法的规定进行测定。染色按GB/T2374—2017的有关规定进行染色。染色用棉布：质量为5g,浴比为1:40,染色浓度为2%(owf),染色温度为70℃。6.4.1.2.1以质量为5g棉布或棉纱染色为例，染液配方见表3。如用质量为10g棉纱，表3中染料用量增加一倍。表3染液配方染杯编号12345染料标准品的质量/g0.09500.10000.1050一一染料样品的质量/g一一一0.10000.10505g/L的柠檬酸溶液体积/mL2222250g/L的明矾溶液体积/mL11111试验用水/mL6.4.1.2.2染色工艺路线见图1。70℃×45min60℃染料10min40℃0.5℃/min0.5℃/min0.8℃/minT/CTES1037—20214将染色后的染样用水洗净后，置于含中性皂2g/L的溶液中，按浴比1:20,70℃煮15min,取出，用水洗净，晾干或60℃以下烘干，水洗和皂洗工艺路线见图2。中性皂水洗10min中性皂70℃×15min图2水洗和皂洗工艺路线6.4.2色光和强度的评定按GB/T2374—2017中第7章的有关规定对染样进行评定。6.5天然性的测定茜草染料中主要成分为茜素，分子结构是1,2-二羟基蒽醌1,2-二羟基9,10-蒽醌，检测织物中是否含有茜素，是鉴别茜草染料染色的理论基础。均匀剪取染色织物试样20g,分5次用100倍(即浴比1:100)50℃温水洗涤，每次5min;再分5次用100倍(即浴比1:100)50℃乙醇洗涤，每次5min;然后烘干，剪成5mm×5mm的小片，混合均匀(称为混合样)。将上述混合样装入250mL圆底烧瓶，加入甲醇100mL,4mol/L盐酸20mL,80℃磁力搅拌加热回流2h,冷却至室温，减压抽滤，得到试样的染料萃取液。将其置于真空旋转蒸发器上，于(50±1)℃温度下低真空浓缩旋干，然后50℃真空干燥24h,得到粉末状固体。6.5.3薄层色谱测试法称取1g茜草染料，放入50mL二氯甲烷溶液中溶解1h～2h后过滤。展开体系体积比：苯：四氯化碳：醋酸：醋酸乙酯=50:75:3.5:8.0。用移液枪吸取适量的展开液点样在硅胶板上，硅胶板放置展开剂中展开15min观察硅胶板斑点颜色情况。经展开的硅胶板上有显示红色斑点，说明产品中含有茜素，判断该产品为植物茜草染料。反之，没有红色斑点显示，说明产品不含茜素，不是植物茜草染料。T/CTES1037—20215液相色谱/质谱联用测试方法见附录A。6.5.5碳14法鉴别仲裁时，按T/CTES1023—2020的4.1.2规定进行鉴别。6.6有害芳香胺的量的测定按照GB19601、GB/T24101的规定进行测定。6.7重金属元素的量的测定按照GB20814的规定进行测定。6.8在纯棉织物上色牢度的测定色牢度的测试样应按GB/T4841.1的规定染成1/1染色标准深度。耐皂洗色牢度按GB/T3921—2008的规定进行测定。采用两块单纤维贴衬织物：其中一块为棉，另一块为羊毛。试样制备按GB/T3921—2008中6.1b)规定进行制备。耐汗渍色牢度按GB/T3922的规定进行测定。耐摩擦色牢度按GB/T3920的规定进行测定。耐水洗色牢度按GB/T5713的规定进行测定。7.1.1每批产品由生产厂的质量检验部门进行检验合格，并附合格证明后方可出厂。生产厂应保证所有出厂的茜草染料都符合本文件要求。7.2.1型式检验的样品应从出厂检验合格的产品中抽取。7.2.2型式检验项目为全项目检验，有下列情况之一进行型式检验：a)新产品鉴定时；T/CTES1037—20216b)停产超过1个月恢复生产时；c)配方、工艺有较大改变，可能影响产品性能时；d)国家质量监督检验部门提出型式检验要求时。如果检验结果中有一项指标不符合本文件的规定时，应重新自两倍量的包装中取样进行重新检验，检验的结果即使只有一项指标不合格，则整批产品不合格。8.1标志茜草染料的每个包装上应有产品名称、型号、厂名、厂址、生产日期、有效期、生产批号、标准编号、净重等标志。本产品外包装用塑料桶，内用塑料袋，加盖密封。每桶净重25kg,其他包装可与客户协商确定。运输过程中应防止暴晒、受潮和碰撞。本产品应贮存在阴凉、干燥、通风的仓库内。T/CTES1037—20217(规范性)液相色谱/质谱联用仪测试法A.1原理茜草染料中主要为茜素，分子结构是1,2-二羟基-9,10-蒽醌(CAS号：72-48-0),还含有少量的大叶茜草素、羟基茜草素、甲基异茜草素，检测织物中是否含有茜素等是鉴别茜草染料染色的理论基础。依据液相色谱/质谱联用分析原理，选用适当的溶剂萃取染色针织服装上的染料，通过与标准样品茜素等保留时间和质谱谱图的比较，检测到识别结构中的茜素等，可判定为茜草染料，由此进行茜草染料的鉴定。A.2试剂A.2.1液相色谱使用的溶剂为色谱纯甲醇。A.2.2三级水，符合GB/T6682的要求。A.2.3浓盐酸、乙酸乙酯、茜素，均为分析纯。A.2.4茜素标准储备溶液(1000mg/L)。用甲醇将茜素配制成浓度约为1000mg/L的储备溶液。A.2.5茜素标准工作溶液(20mg/L)。从标准储备溶液中取0.2mL置于容量瓶中，用甲醇定容至A.3设备和仪器液相色谱/质谱联用仪：配二极管阵列检测器和XCT型离子阱质量检测器。A.4液相色谱/质谱联用定性鉴别A.4.1分析条件A.4.1.1液相色谱分析条件如下：a)色谱柱：ZORBAXEclipseXDB-C₁84.6mm×150mm,5μm;b)流动相：乙腈(A):0.1%甲酸水溶液(B)或甲醇(C):水(D)/0.2%甲酸水溶液(E);c)柱温：30℃;d)检测器：DAD(190nm～800nm);e)检测波长：395nm;f)流速：0.8mL/min;A.4.1.2质谱分析条件如下：a)进样方式：LC-MS;b)离子源：ESI;c)检测模式：负离子；d)扫描范围(m/z):20～1500;e)离子源温度：280℃;f)雾化气流速：40psi(275.8kPa);g)干燥气流速：10L/min;T/CTES1037—20218h)毛细管电压：3500V;A.4.2鉴别配制20mg/L的茜草样品溶液，取上清液，注入色谱仪，按照A.4.1条件操作。通过比较试样与标准样品茜素的保留时间和质谱图，鉴别织物是否为茜草染料染色产品。A.4.3与合成染料的识别若试样液相图谱中有明显出峰，且保留时间及质核比与茜素标准品提供的液相-质谱联用谱图不同，则认为织物中含有合成染料或本文件规定以外的植物染料。经液相色谱/质谱联用图谱检测，茜素的标准品和茜草染料染色织物样品的谱图见图A.1～图A.4。图A.1茜素标准品液相谱图Intens2.52.00.50.0-注：检测模式：负离子；离子源温度：280℃。图A.2200茜素标准品质谱图238.4250300m/:9图A.3茜草染料染色织物样品液相谱图64202002250图A.4茜草染料染色织物样品质谱图ICS87.060.10CCSG57T/CTES1037—2021Vegetabledyesfortextiles—纺织用植物染料茜草染料Issuedate:2021-03-17Implementationdate:2021-04-16IsseudbyChinaTextileEngineeringSocietyT/CTES1037—2021ForewordThisdocumentisdraftedinaccordancewiththerulesofGB/T1.1—2020Directivesforstandardiza-tionPart—1:Rulesforthestructureanddraftingofstandardizingdocuments.Attentionsisdrawntothepossibilitythatsomeoftheelementsofthestandardmaybesubjectofpatentrights.Theissuingbodyofthisdocumentshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.ThisdocumentwasproposedbyStandardizationTechnicalCommitteeofChinaTextileEngineeringSociety.ThisdocumentisunderChinaTextileEngineeringSociety.ThisdocumentwasresponsiblydraftedbyWuhanTextileUniversityandChangzhouUniversity.ThisdocumentwasdraftedbyYantaiMingyuanHomeTextileCo.,Ltd.,GuangdongYidaTextileCo.,Ltd.,AidaCo.,Ltd.,ZiboXiangyuanTextileCo.,Ltd.,Chongqing35333PrintingandDyeingGarmentGeneralFactoryCo.,Ltd.,DezhouHengfengTextileCo.,Ltd.,XiamenXtepChildren'sProductsCo.,Ltd.Chiefdraftingstaffofthisdocument:JiangHuiyu,JiJunling,XueZhiyong,ZhouLiming,YaoJinbo,LiWenwei,WangWen,ZhouXuanLi,QinXiaoxia,LiuYuqing,LiSuhong,SunYing,YangHong,ZhiJun,BaiMeng,XuMing,WangZhi.Vegetabledyesfortextiles—Thisdocumentspecifiesthedefinition,requirements,sampling,testmethods,inspectionrulesaswellasmarking,packaging,transportationandstorageofvegetablemadderdyes.Thisdocumentisapplicabletoplantdyesderivedfrommadderplantsources.2NormativereferencesThefollowingreferenceddocumentsareindispensablefortheapplicationofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,thelatesteditionsofthedocumentofthenormativedocuments(includingalltheamendments)areapplicabletothisdocument.GB/T2386—2014Dyesanddyeintermediates—DeterminationofmoistureGB/T2390Dyes—DeterminationofpHvalueGB/T3920Textile—Colourfastnesstest—ColourfastnesstorubbingGB/T3921—2008Textile—Colourfastnesstest—ColourfastnesstosoapwashingGB/T3922Textile—Colourfastnesstest—ColourfastnesstoperspirationGB/T4841.1Standarddepthcolorcard1/1T/CTES1037—2021GB/T5713TextileColourfastnesstest—ColorfastnesstowashingGB/T6678—2003GeneralrulesforsamplingofchemicalproductsGB/T6682WaterspecificationsandtestmethodsforanalyticalexperimentalGB19601Limitationanddeterminationof23harmfularomaticaminesindyeproductsGB20814LimitationanddeterminationofheavymetalelementsindyeproductsGB/T24101Limitationsanddeterminationof4-aminoazobenzeneindyeproductsT/CTES1023—2020Methodsforidentificationofbiomasspropertiesoftextileauxiliaries一3TermsanddefinitionsThefollowingtermsanddefinitionsapplyforpurposesofthisdocument.rubiacordifoliaThemaincompositionofmadderdyeisalizarin,itschemicalname:1,2-dihydroxyanthraquinone1,2-dihydroxy-9,10-anthraquinone;Molecularformula:C14H8O4relativemolecularweight240.21;CAS:72-48-0;Molecularstructureformula:3.2naturalityThedyeisextractedfromtherootsandstemsofmadderplantscontaininganthraquinonederivativesanddoesnotcontainanychemicalsyntheticorganicmatter.4Requirements4.1ThequalityofmadderdyeshallmeettherequirementsofTable1.T/CTES1037—2021Table1—QualityrequirementsofmadderdyesProjectsIndicatorsAppearanceMagentauniformpowderpHvalue5.5～6Themassfractionofmadderdye/%Massfraction/%oflowboilingpointvolatilesIntensity(points)Comparewithstandardproducts100ComparewithstandardproductssimilarNaturalityCharacteristicsofalizarinMassfractionofharmfularomaticamines/(mg/kg)ItshallbeexecutedaccordingtoGB19601andGB/T24101Themassfractionofheavymetalelements/(mg/kg)ItisshallbeperformedaccordingtoGB208144.2Thedyeingpropertiesandfastnessofmadderdyesoncottonfabricsshallconformtotheprovi-sionsinTable2.Table2—DyeingpropertiesandfastnessofmadderdyesoncottonfabricsUnit:grade35ThesamplingSamplesaretakeninbatches,andabatchofevenlymixedproductsistakenastheproductionplant.Thenumberofsamplesshallbeinaccordancewith7.6inGB/T6678—2003.Thepackageofthesam-pledproductshouldbeingoodcondition,andtheexternalimpuritiesshouldnotfallintotheproductduringsampling.Duringsampling,theprobetubeshalltakethesamplesofupper,middleandlowerparts,andtheweightofthesamplesshallnotbelessthan500g.Afterthoroughlymixingthesamplestaken,dividethemintotwoclean,dry,wellsealedcontainerswithlabelsattachedtothem.Indicate:productname,batchnumber,nameofmanufacturer,dateandplaceofsampling.Oneforinspectionandoneforfuturereference.T/CTES1037—20216Testmethods6.1AppearanceVisualassessmentwasperformedundernaturallight.6.2DeterminationofpHvalueAccordingtoGB/T2390.6.3DeterminationofvolatilesatlowboilingpointAccordingtotheprovisionsof3.2dryingmethodinGB/T2386—2014.6.4Determinationofintensityandcolorlight6.4.1Dyeingmethod(arbitrationtestmethod)6.4.1.1GeneraldyeingconditionsAccordingtorelevantregulationsofGB/T2374—2017.Weightofcotton:5g;bathratio:1:40;Dyeingconcentration:2%(owf);dyeingtemperature:70℃.6.4.1.2Formulaofdyeingliquorandrouteofdyeingprocess6.4.1.2.1Take5gcottonorcottonyarndyeingasanexample,theformulaofdyeingsolutionisshowninTable3.If10gcottonyarnisused,theamountofdyeinTable3isdoubled.Table3—FormulationofdyesolutionThenumberofthedyeingcup12345Qualityofdyestandard/g0.09500.10000.1050一一Themassofthedyesample/g一一一0.10000.1050Volumeofcitricacidsolution(5g/L/mL22222Volumeofalumsolution(50g/L)/mL11111Volumeofwaterusedinthetest/mLT/CTES1037—20216.4.1.2.2DyeingprocessissFigure1—Dyeingprocess6.4.1.3WashingandsoapingThedyedsampleswerewashedwithwater,placedinasolutioncontaining2gofneutralsoapperli-ter,boiledatabathratioof1:20and70℃for15min,andthentakenoutandwashedwithwater.Finally,thesamplesweredryordriedbelow60℃.TheprocessofwashingandsoapingareshowninFigure2.Figure2—Washingandsoapingprocess6.4.2EvaluationofcolorlightandintensityThedyedsampleswereevaluatedaccordingtotherelevantprovisionsofChapter7ofGB/T2374—2017.6.5Determinationofnaturalproperties6.5.1MechanismThemaincomponentofmadderdyeisalizarin,whosemolecularstructureis1,2-dihydroxyanthra-quinone1,2-dihydroxyanthraquinone9,10-anthraquinone.Thedetectionofalizarininfabricisthetheoreticalbasisforidentifyingmadderdye.6.5.2StrippingofdyeThedyedfabricsample(20g)wasevenlycutandwashedinwarmwaterat50℃(bathratio1:100,time:5min)for5times;Thenwashwithethanolat50℃for5times(bathratio1:100,time:5in);Thendry,cutinto5mm×5mmpieces,andmixwell(calledmixingsample).Puttheabovemixedsamplesintoa250mLround-bottomedflask,add100mLmethanoland20mL4mol/LT/CTES1037—2021hydrochloricacid.Then,thesamplewasmagneticallystirredat80℃for2h(withrefluxdevice),andfinallycooledtoroomtemperature.Aftervacuumpumpingandfiltration,thedyeextractionso-lutionofthesamplewasobtained.Theextractwasconcentratedinavacuumrotaryevaporatorat(50±1)℃,andthendriedinavacuumdryingovenat50℃for24h.Finally,thepowdersolidwasobtained.6.5.3Thinlayerchromatography6.5.3.1PreparationofsamplesolutionWeighed1gmadderdyeanddissolveditin50mLdichloromethanesolutionfor1h~2hbeforefil-tration.6.5.3.2PreparationofdevelopingagentThevolumeratioofdevelopedsystem:benzene:carbontetrachloride:aceticacid:ethylacetate=50:75:35:8.0.6.5.3.3ObservationAnappropriateamountofthedevelopingsolutionwasabsorbedonthesilicagelplatewithapipettegun,andthenplacedinthedevelopingagentfor15min,andthecolorofspotsonthesilicagelplatewasobserved.6.5.3.4ResultsThereareredspotsonthesilicagelplate,indicatingthattheproductcontainsalizarin,judgingthattheproductisplantalizarindye.Onthecontrary,thereisnoredspots,indicatingthattheproductdoesnotcontainalizarin,notmadderplantdye.ThemethodisshowninAppendixA.6.5.5C14identificationArbitrationshallbeconductedinaccordancewith4.1.2ofT/CTES1023—2020.6.6DeterminationofharmfularomaticaminesInaccordancewithGB19601,GB/T24101.T/CTES1037—20216.7DeterminationoftheamountofheavymetalsInaccordancewithGB20814.6.8Determinationofcolourfastnesstocottonfabrics6.8.1GeneralprovisionsAllsamplesforcolorfastnessshallbedyedto1/1standardstainingdepthasspecifiedinGB/T4841.1.6.8.2DeterminationofcolourfastnesstowashingColourfastnesstowashingshallbecarriedoutaccordingtoGB/T3921—2008.Preparetwomonofilamentliningfabrics:Oneiscotton,theotheriswool.Thesamplepreparationwascarriedoutaccordingtotheprovisionsof6.1b)inGB/T3921—2008.6.8.3DeterminationofcolourfastnesstoperspirationColourfastnesstoperspirationisaccordingtoGB/T3922.6.8.4DeterminationofcolourfastnesstorubbingColourfastnesstofrictionshallbecarriedoutaccordingtoGB/T3920.6.8.5ColorfastnesstowashingThecolorfastnesstowashingshallbecarriedoutaccordingtoGB/T5713.7.1Thefactoryinspection7.1.1Eachbatchofproductsshallbeinspectedbythequalityinspectiondepartmentofthemanu-facturerandattachedwiththecertificatebeforeleavingthefactory.Themanufacturershallensurethatallmadderdyesproducedbythefactorymeettherequirementsofthisdocument.20T/CTES1037—20217.1.2Ex-factoryinspectionitems:Appearance,madderdyemassfraction,moisturemassfraction,colorfastnessandnatural.7.2Typeinspection7.2.1Thesamplesfortypeinspectionshouldbeselectedfromtheproductsthatpassthefactoryinspection.7.2.2Typeinspectionitemisthewholeprojectinspection,typeinspectioniscarriedoutinoneofthefollowingsituations:a)Newproductidentification;b)Whentheproductionisresumedaftermorethanonemonth;c)Whentheformulaandprocessaregreatlychanged,whichmayaffecttheperformanceoftheproduct;d)Whenthenationalqualitysupervisionandinspectiondepartmentputsforwardthetypeinspec-tionrequirements.7.3ThereinspectionIfoneoftheinspectionresultsdoesnotconformtotherequirementsofthisdocument,samplesshouldbetakenfromtwicetheamountofpackagingforinspection.Ifonlyoneoftheinspectionre-sultsfails,thewholebatchofproductsisnotqualified.8Marking,packaging,transportationandstorage8.1MarkingEachpackageofmadderdyestuffshallbemarkedwiththeproductname,modelnumber,factoryname,factoryaddress,productiondate,expirationdate,productionbatchnumber,standardnum-ber,netweight,etc.8.2PackagingTheouterpackingofthisproductisplasticbucket,innerplasticbag,sealedwithcap.Thenetweightofeachbarrelis25kg.Otherpackingcanbedeterminedbynegotiationwiththecustomer.218.3TransportationExposure,dampnessandcollisionshouldbeprotectedduringtransportation.8.4StorageThisproductshouldbestoredinacool,dryandventilatedwarehouse.22T/CTES1037—2021AppendixA(Normative)MethodofliquidchromatographycombinedwithmassspectrometryThemainmadderdyeisalizarin,whosemolecularstructureis1,2-dihydroxy-9,10-anthraquinone(CAS:72-48-0),andalsocontainsasmallamountofmaddermacrophylla,hydroxy-alizarin,methyliso-alizarin.Thedetectionofalizarininfabricisthetheoreticalbasisfortheidentificationofmadderdye.Accordingtotheprincipleofliquidchromatography-massspectrometry(LC-MS),appropriatesolventwasselectedtoextractthedyesfromknittinggarments,andthealizarinintherecognitionstructurewasdetectedbycomparingtheretentiontimewiththestandardsampleandthemassspec-trum,andthealizarinintherecognitionstructurecouldbedeterminedasalizarindyestuff,thusthealizarindyestuffwasidentified.A.2AgentsA.2.1Thesolventusedforliquidchromatographywaspuremethanol.A.2.2Tertiarywater.MeettherequirementsofGB/T6682.A.2.3Concentratedhydrochloricacid,ethylacetateandalizarinwereallanalysicallypure.A.2.4Alizarinstandardreservesolution(1000mg/L).Alizarinwaspreparedwithmethanolintoareservesolutionwithaconcentrationofabout1000mg/L.A.2.5Alizarinstandardworkingsolution(20mg/L).0.2mLofthestandardreservesolutionwasplacedinavolumetricflaskandvolumetizedto10mLwithmethanol.A.3EquipmentandinstrumentsLiquidchromatographycombinedwithmassspectrometer:withdiodearraydetectorandXCTiontrapmassdetector.23T/CTES1037—2021A.4QualitativeidentificationbyliquidchromatographycombinedwithmassspectrometryA.4.1ThetestconditionsA.4.1.1Theliquidchromatographytest