DB43-T 3084-2024.舒緩、修護(hù)類(lèi)化妝品中52種抗過(guò)敏成分的測(cè)定+++液相色譜串聯(lián)質(zhì)譜法

ICS01.040.11CCSICS01.040.11CCSC50湖 南 省 地 方 標(biāo) 準(zhǔn)DB43/T3084—2024舒緩、護(hù)類(lèi)化品中52種抗過(guò)敏分測(cè)定 液相色譜聯(lián)質(zhì)譜法Detectionof52rohibitedanti-allergicingredientsinsoothingandDetectionof52rohibitedanti-allergicingredientsinsoothingandrepairingcosmetics-Liquidchromatography-tandemmassspectrometry2024111320250213湖南省市場(chǎng)監(jiān)督管理局發(fā)布目 次前言 II1范引文件 1語(yǔ)定義 1法1劑材料 1通要求 1試劑 2試配制 2標(biāo)物質(zhì) 2標(biāo)儲(chǔ)溶配制 2材料 2儀和2析2篩用合準(zhǔn)2空基提液2基混標(biāo)中制備 3基混系標(biāo)液的3樣處理 3儀參條件 3定判定 7定測(cè)定 7空試驗(yàn) 7果7敏度 7密度 9附錄A（料）52抗過(guò)成的文稱(chēng)英文稱(chēng)CAS號(hào)分10附錄B（料）52抗過(guò)成提離12前 言本文件按照GB/T1.1—2020《標(biāo)準(zhǔn)化工作導(dǎo)則第1部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》的規(guī)定起草。請(qǐng)注意本文件的某些內(nèi)容可能涉及專(zhuān)利。本文件的發(fā)布機(jī)構(gòu)不承擔(dān)識(shí)別專(zhuān)利的責(zé)任。本文件由湖南省藥品監(jiān)督管理局提出并歸口。本文件起草單位：湖南省藥品檢驗(yàn)檢測(cè)研究院、水羊化妝品制造有限公司。舒緩、修護(hù)類(lèi)化妝品中52種抗過(guò)敏成分的測(cè)定 液相色譜串聯(lián)譜法范圍本文件規(guī)定了舒緩修護(hù)類(lèi)化妝品中52種抗過(guò)敏成分高效液相色譜串聯(lián)質(zhì)譜法。52文件。GB/T6682分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法3術(shù)語(yǔ)和定義下列術(shù)語(yǔ)和定義適用于本文件。舒緩類(lèi)化妝品soothingcosmetics有助于改善皮膚刺激等狀態(tài)的化妝品。修護(hù)類(lèi)化妝品repairingcosmetics文件。GB/T6682分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法3術(shù)語(yǔ)和定義下列術(shù)語(yǔ)和定義適用于本文件。舒緩類(lèi)化妝品soothingcosmetics有助于改善皮膚刺激等狀態(tài)的化妝品。修護(hù)類(lèi)化妝品repairingcosmetics有助于維護(hù)施用部位保持正常狀態(tài)的化妝品。4方法原理相對(duì)豐度比定性、定量離子對(duì)峰面積定量，以標(biāo)準(zhǔn)曲線(xiàn)法計(jì)算含量。5試劑與材料通用要求GB/T6682試劑50%70%7:30.12mmol/L0.1261g1000mL950mL1.0mL0.22μm本方法所包含的52種抗過(guò)敏成分標(biāo)準(zhǔn)品的中文名稱(chēng)、英文名稱(chēng)、CAS號(hào)、分子式詳見(jiàn)附錄A的表A.1。A.1）10mg（0.00001g）mL43材料材料：15mL。：3mL。0.22μm：25mL。儀器和設(shè)備5.7.1液相色譜-三重四極桿質(zhì)譜聯(lián)用儀：配有電噴霧離子源（ESI）。5.7.20.0001g0.00001。6000r/min。200W。6分析步驟524）0.20.000125mL1.0mL，100mL10.0mg/L1.02.05.010.020.0、50.0μg/L0.2g（0.0001g）25mL1～2mL30s20min6000r/min10min（50%0.22μm）后加入70%乙腈3mL，渦旋振蕩2min，6000r/min離心10min，吸取下層溶液至25mL具塞比色管70后加入70%乙腈3mL，渦旋振蕩2min，6000r/min離心10min，吸取下層溶液至25mL具塞比色管703250500.22μm）儀器參考條件a)色譜柱：C18（100mm×2.1mm，1.8μm），或相當(dāng)者；：40：2μL；流速：0.3mL/min；。表1液相色譜梯度洗脫條件時(shí)間min流動(dòng)相A（含0.1%甲酸的2mmol/L甲酸銨水溶液）%流動(dòng)相B（甲醇）%0.080201.080202.540603.520806.01998.019913.0802015.08020（ESI）；（MRM）；2。表252序號(hào)名稱(chēng)保留時(shí)間min母離子m/z子離子m/z碰撞能eV1布可立嗪6.25433.2201.0*27433.2166.0612卡比沙明5.28291.1202.0*21291.1167.0423氯苯甲嗪5.64301.1201.0*18301.1166.0424奧沙米特5.57427.2167.0*30427.2259.0245苯噻啶5.59296.196.0*27296.1199.0346苯托沙敏5.51256.172.0*23256.157.0557氮異丙嗪5.40286.1241.0*21286.1199.0478多塞平5.44280.1235.0*23280.1107.0279甲吡吩嗪5.60297.198.0*25297.1266.02510雷尼替丁4.42315.1176.0*23315.1102.04811氯吡拉敏5.45290.1125.0*40290.1245.02012溴苯海明5.63334.0245.0*17334.0166.04013異丁嗪5.60299.2100.0*24299.2212.03014苯吡丙胺4.96241.2196.0*20241.2167.05315吡咯咪唑5.53326.1255.0*25326.1220.03116二氧異丙嗪5.04317.186.0*25317.1272.027表252種抗過(guò)敏成分監(jiān)測(cè)離子對(duì)及相關(guān)參數(shù)設(shè)定表表252種抗過(guò)敏成分監(jiān)測(cè)離子對(duì)及相關(guān)參數(shù)設(shè)定表（續(xù)）序號(hào)名稱(chēng)保留時(shí)間min母離子m/z子離子m/z碰撞能eV17法莫替丁4.43338.0259.0*16338.0189.02518美克洛嗪5.93391.2201.0*24391.2166.05319美吡拉敏5.21286.2121.0*27286.2241.02120腦益嗪5.76369.2167.0*21369.2201.01621去氯羥嗪5.43341.2167.0*24341.2152.06922西咪替丁4.46253.1159.0*20253.1117.02123安他唑啉5.36266.291.0*32266.2196.02224地氯雷他定5.44311.1259.0*29311.1243.06325氯苯那敏5.30275.1230.0*21275.1167.05126西替利嗪5.88389.2201.1*25389.2165.07727阿司咪唑5.18459.2135.0*41459.2218.03528曲吡那敏5.22256.2211.0*20256.2119.03829溴苯那敏5.35319.0167.0*52319.0194.05830苯海拉明5.39256.1167.0*18256.1152.04831異丙嗪5.52285.186.0*20285.1198.02932羥嗪5.62375.2201.0*24375.2166.05133奮乃靜5.87404.1171.0*32404.1143.03634氟奮乃靜5.92438.1171.0*33438.1143.03935氯丙嗪5.76319.186.0*24序號(hào)名稱(chēng)保留時(shí)間min母離子m/z子離子m/z碰撞能eV319.158.06036氯雷他定6.84383.1337.0*31383.1267.04337特非那定5.88472.4436.0*36472.457.08538賽庚啶5.58288.2191.0*39288.296.03039多拉西敏4.93271.2182.0*23271.2167.04440氯苯沙明5.66304.1215.0*17304.190.01141美沙吡林5.13262.1217.0*18262.197.05242賽克利嗪5.43267.2167.0*20267.2165.05243二苯拉林5.49282.2167.0*28282.2116.03944非索非那定5.51502.3466.0*39502.3171.04645阿伐斯汀5.44349.2278.0*21349.2232.04646咪唑斯汀5.41433.2308.0*33433.2254.04247依巴斯汀6.16470.3167.0*33470.3203.03848奧洛他定5.26338.2247.0*30338.2165.03149盧帕他定5.54416.2309.0*25416.2282.02950貝托斯汀5.34389.2202.0*28389.2170.02851比拉斯汀5.40464.3272.0*50464.3191.05252酮替芬5.16310.196.0*29310.1213.039注1：*表示定量離子。注2：52種抗過(guò)敏組分提取離子圖見(jiàn)附錄B的圖B.1至圖B.52。取待測(cè)溶液與篩查用混合標(biāo)準(zhǔn)溶液在相同分析條件下測(cè)定，樣品中如呈現(xiàn)定量離子對(duì)和定性離子3的規(guī)定，表3定性判定時(shí)離子相對(duì)豐度的最大允許偏差離子相對(duì)豐度（k）k＞50%50%≥k＞20%20%≥k＞10%k≤10%允許的最大偏差±20%±25%±30%±50%0.99。待測(cè)溶液中各組分的響應(yīng)值應(yīng)在儀器線(xiàn)性響應(yīng)范圍內(nèi)。若待測(cè)溶液響應(yīng)值超出基質(zhì)標(biāo)準(zhǔn)曲線(xiàn)線(xiàn)性范圍，應(yīng)用空白基質(zhì)樣液將其稀釋至線(xiàn)性范圍內(nèi)進(jìn)行定量測(cè)定。測(cè)定結(jié)果按公式（1）計(jì)算樣品中各成分的含量。除不加試樣外，按6.1至6.5項(xiàng)下的測(cè)定條件和步驟進(jìn)行。7結(jié)果計(jì)算7結(jié)果計(jì)算（1）52????=????×????×????···········································································(1)式中：ω——樣品中52種抗過(guò)敏類(lèi)成分的質(zhì)量分?jǐn)?shù)，μg/g；????——待測(cè)溶液中52種抗過(guò)敏成分的質(zhì)量濃度，μg/L；V——樣品定容體積，mL；m——樣品取樣量，g；D——稀釋倍數(shù)（如未稀釋則為1）。8靈敏度520.2g表4。表452種抗過(guò)敏類(lèi)成分的檢出限、定量限、檢出濃度和最低定量濃度序號(hào)化合物名稱(chēng)檢出限μg/L定量限μg/L檢出濃度μg/g最低定量濃度μg/g1布可立嗪0.0010.0020.250.502卡比沙明0.0010.0020.250.50表452種抗過(guò)敏類(lèi)成分的檢出限、定量限、檢出濃度和最低定量濃度表452種抗過(guò)敏類(lèi)成分的檢出限、定量限、檢出濃度和最低定量濃度（續(xù)）序號(hào)化合物名稱(chēng)檢出限μg/L定量限μg/L檢出濃度μg/g最低定量濃度μg/g3氯苯甲嗪0.0010.0020.250.504奧沙米特0.0010.0020.250.505苯噻啶0.0010.0020.250.506苯托沙敏0.0010.0020.250.507氮異丙嗪0.0010.0020.250.508多塞平0.0010.0020.250.509甲吡吩嗪0.0010.0020.250.5010雷尼替丁0.0010.0020.250.5011氯吡拉敏0.0010.0020.250.5012溴苯海明0.0010.0020.250.5013異丁嗪0.0010.0020.250.5014苯吡丙胺0.0010.0020.250.5015吡咯咪唑0.0010.0020.250.5016二氧丙嗪0.0010.0020.250.5017法莫替丁0.0010.0020.250.5018美克洛嗪0.0010.0020.250.5019美吡拉敏0.0010.0020.250.5020腦益嗪0.0010.0020.250.5021去氯羥嗪0.0010.0020.250.5022西咪替丁0.0010.0020.250.5023安他唑啉0.0010.0020.250.5024地氯雷他定0.0010.0020.250.5025氯苯那敏0.0010.0020.250.5026阿司咪唑0.0010.0020.250.5027曲吡那敏0.0010.0020.250.5028溴苯那敏0.0010.0020.250.5029苯海拉明0.0010.0020.250.5030異丙嗪0.0010.0020.250.5031羥嗪0.0010.0020.250.5032奮乃靜0.0010.0020.250.5033西替利嗪0.0010.0020.250.5034氟奮乃靜0.0010.0020.250.5035氯丙嗪0.0010.0020.250.5036氯雷他定0.0010.0020.250.5037特非那定0.0010.0020.250.5038賽庚啶0.0010.0020.250.5039多西拉敏0.0010.0020.250.50序號(hào)化合物名稱(chēng)檢出限μg/L定量限μg/L檢出濃度μg/g最低定量濃度μg/g40氯苯沙明0.0010.0020.250.5041美沙吡林0.0010.0020.250.5042賽克利嗪0.0010.0020.250.5043二苯拉林0.0010.0020.250.5044非索非那定0.0010.0020.250.5045阿伐斯汀0.0010.0020.250.5046咪唑斯汀0.0010.0020.250.5047依巴斯汀0.0010.0020.250.5048奧洛他定0.0010.0020.250.5049盧帕他定0.0010.0020.250.5050貝托斯汀0.0010.0020.250.5051比拉斯汀0.0010.0020.250.5052酮替芬0.0010.0020.250.509精密度15%。附錄A（資料性）52種抗過(guò)敏成分的中文名稱(chēng)、英文名稱(chēng)、CAS號(hào)及分子式52種抗過(guò)敏成分的中文名稱(chēng)、英文名稱(chēng)、CAS號(hào)及分子式見(jiàn)表A.1。表A.152種抗過(guò)敏成分的中文名稱(chēng)、英文名稱(chēng)、CAS號(hào)及分子式序號(hào)中文名稱(chēng)英文名稱(chēng)CAS號(hào)分子式1布可立嗪Buclizine82-95-1C28H33ClN22卡比沙明Carbinoxamine486-16-8C16H19ClN2O3氯苯甲嗪Meclizine82-93-9C18H21ClN24奧沙米特Oxatomide60607-34-3C27H30N4O5苯噻啶Pizotifen15574-96-6C19H21NS6苯托沙敏Phenyltoloxamine92-12-6C17H21NO7氮異丙嗪Isothipendyl482-15-5C16H19N3S8多塞平Doxepin1668-19-5C19H21NO9甲吡吩嗪Methdilazine1982-37-2C18H20N2S10雷尼替丁Ranitidine66357-35-5C13H22N4O3S11氯吡拉敏Chloropyramine59-32-5C16H20ClN312溴苯海明Bromazine118-23-0C17H20BrNO13異丁嗪Trimeprazine84-96-8C18H22N2S14苯吡丙胺Pheniramine86-21-5C16H20N215吡咯咪唑Clemizole442-52-4C19H20ClN316二氧丙嗪Dioxopromethazine13754-56-8C17H20N2O2S17法莫替丁Famotidine76824-35-6C8H15N7O2S318美克洛嗪Meclozine569-65-3C25H27ClN219美吡拉敏Pyrilamine91-84-9C17H23N3O20腦益嗪Stugeron298-57-7C26H28N221去氯羥嗪Decloxizine3733-63-9C21H28N2O222西咪替丁Cimetidine51481-61-9C10H16N6S23安他唑啉Antazoline91-75-8C17H19N324地氯雷他定Desloratadine100643-71-8C19H19ClN225氯苯那敏Chlorpheniramine131-73-7C16H19ClN226阿司咪唑Astemizole68844-77-9C28H31FN4O27曲吡那敏Tripelennamine91-81-6C16H21N328溴苯那敏Brompheniramine86-22-6C16H19BrN229苯海拉明Diphenhydramine58-73-1C17H21NO30異丙嗪Promethazine60-87-7C17H20N2S31羥嗪Hydroxyzine68-88-2C21H27ClN2O2表A.152CAS（序號(hào)中文名稱(chēng)英文名稱(chēng)CAS號(hào)分子式32奮乃靜Perphenazine58-38-8C21H26ClN3OS33西替利嗪Cetirizine83881-51-0C21H25ClN2O334氟奮乃靜Fluphenazine69-23-8C22H26F3N3OS35氯丙嗪Chlorpromazine50-53-3C17H19ClN2S36氯雷他定Loratadine79794-75-5C22H23ClN2O237特非那定Terfenadine50679-08-8C32H41NO238賽庚啶Cyproheptadine129-03-3C21H21N39多西拉敏Doxylamine469-21-6C17H22N2O40氯苯沙明Chlorphenoxamine77-38-3C18H22ClNO41美沙吡林Methapyrilene91-80-5C14H19N3S42賽克利嗪Cyclizine82-92-8C18H22N243二苯拉林Diphenylpyraline147-20-6C19H23NO44非索非那定Fexofenad