CN112834642A - 高油复杂基质样品前处理技术结合uplc-msms测定191种农药残留的方法 - Google Patents
高油复杂基质样品前处理技术结合uplc-msms测定191种农药残留的方法 Download PDFInfo
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Abstract
本发明提供一种高油复杂基质样品前处理技术结合UPLC‑MSMS测定191种农药残留的方法,称取适量高油复杂基质样品于离心管外萃取管中,加入超纯水、乙酸酸化乙腈、陶瓷均质子和萃取盐,内插管中加入萃取盐、净化剂和陶瓷均质子,把内插管嵌套入外萃取管中拧好,置于全自动样品处理设备,经反复震荡、多次离心处理后,取内插管中适量上清液,氮吹至近干,加入1ml乙腈:水(3:2)超声复溶,过0.22μm滤膜,利用UPLC‑MS/MS实现191种农药残留的检测。各农药组分在色谱柱下分离效果好,所测得的检出限、定量限等各项指标满足农药的多残留分析,可以应用于高油复杂基质样品的多农药残留检测中。
Description
技术领域
本发明属于农药残留分析技术领域,具体涉及一种高油复杂基质样品前处理技术结合 UPLC-MSMS测定191种农药残留的方法。
背景技术
农药残留检测技术目前已经在普通果蔬基质发展较为完善,但在一些复杂基质的检测 方法和技术相关发展仍然存在挑战,特别是高油复杂基质样品,含油量高、色素含量大, 还含有多糖、蛋白质等成分,基质成分复杂,目标农药与基质分离难度大,在前处理的过 程中如果无法有效的去除基质所带来的干扰,则会在仪器检测过程中无法实现准确的定性 和定量。
目前对于高油复杂基质农药残留检测技术的研究,仅针对某一类检测对象。由于不同 的高油复杂基质样品中基质种类差别较大,现有样品前处理技术中,针对不同种样品采用 不同的样品前处理方法,需要准备不同的检测试剂、不同的处理流程,不利于降低检测成 本和提高检测人员的熟练程度,目前没有一种通用的、标准化的样品前处理技术可以针对 高油复杂基质样品进行有效地处理。
目前全球已注册的农药超2000余种,其中常用的约500种,而且不断有新的农药被研发和应用。高油复杂基质样品涉及的农药种类也越来越多,但是已有的农药残留检测技术仅能针对少数农药种类进行检测。CN109932467A超高效液相色谱-四级杆/高分辨质谱法测定花生中黄曲霉毒素和农药残留的方法,样品经乙酸-乙腈-水提取液提取、PSA与C18硅胶混合体系净化,正离子模式下使用含0.1%甲酸的水溶液和甲醇为流动相梯度洗脱,高分辨质谱定性定量检测,实现了11种农药残留的检测。目前的检测技术已经不能适应 样品种类众多、农药品种日益增加的现状,不能满足进出口商品对于农药残留检测的需求。
为了解决上述问题,本发明提供一种高油复杂基质样品通用的前处理技术,适用于花 生、花椒、芝麻、八角、桂皮、胡椒、孜然、香叶、陈皮等,能够实现191种目标农药与 基质的有效分离,结合液相色谱串联三重四极杆质谱法(LC-MS/MS),能够对191种农药 实现液相色谱分离,检出限(LOD)范围为1-5μg/kg,定量限(LOQ)范围为2-20μg/kg, 在1倍、2倍和10倍LOQ添加水平下,191种农药的回收率范围分别为70.89-107.6%、 70.49-116.44%和70.88-119.02%,各添加水平相对标准偏差(RSD)均<13.9%。对于填补 高油复杂基质样品多农药残留研究现状的空白,打破进出口贸易壁垒,具有十分重要的意 义。
发明内容
针对上述问题,本发明提供了一种高油复杂基质样品前处理技术结合UPLC-MSMS测 定191种农药残留的方法。
本发明的技术方案是:一种高油复杂基质样品前处理技术结合UPLC-MSMS测定191种农药残留的方法,其特征是,包括以下步骤:
1.高油复杂基质样品前处理过程:
称取适量样品于离心管外萃取管中,加入超纯水、乙酸酸化乙腈、陶瓷均质子和萃取 盐,内插管中加入萃取盐、净化剂和陶瓷均质子,把内插管嵌套入外萃取管中拧好,置于全自动样品处理设备,经反复震荡、多次离心处理后,取内插管中适量上清液,氮吹至近干,加入1ml乙腈:水(3:2)超声复溶,过0.22μm滤膜,待上机检测。
所述高油复杂基质样品为花生、花椒、芝麻、八角、桂皮、胡椒、孜然、香叶、陈皮 中的一种。
所述萃取盐为:无水硫酸镁和氯化钠、乙酸钠、柠檬酸钠、柠檬酸氢二钠的一种或多 种。优选无水硫酸镁和乙酸钠,无水硫酸镁:乙酸钠=4:1,在有效除水的同时,与提取剂形成乙酸-乙酸钠缓冲体系,更加有助于农药的萃取;或优选无水硫酸镁、柠檬酸钠和柠檬酸氢二钠,无水硫酸镁:柠檬酸钠:柠檬酸氢二钠=4:1:1,在有效去除水分的同时,对碱 敏感性农药起到保护作用;或优选无水硫酸镁和氯化钠,无水硫酸镁:氯化钠=2:1在有效 去除水分的同时,使水相与有机相进一步分离。
所述外萃取管所加提取剂为1%乙酸酸化乙腈和超纯水,按体积比计,1%乙酸酸化乙 腈:超纯水=3:2。所述外萃取管中高油复杂基质样品、水、1%乙酸酸化乙腈提取液与萃取 盐的质量体积比为2g:10ml:15ml:7.5g。
所述净化剂为乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合硅胶(C18)、石墨化无孔碳 (ENVI-Carb)、石墨化碳黑(GCB)、多壁碳纳米(Cleaner NANO-carb)、二氧化锆胶(Z-Sep)、 碳十八键合锆胶(Z-Sep+)、弗罗里硅土(Florisil)、增强型脂质去除剂(EMR-Lipid)的一种或多 种。
全自动样品处理程序为①振荡频率1100rpm、振荡10分钟;②4200rpm、离心5分钟;③振荡频率1100rpm、振荡5分钟;4200rpm、离心5分钟。
2.UPLC-MS/MS检测过程:
色谱条件:色谱柱为C18色谱柱,2.1mm×100mm,3.5μm;柱温:40℃;流速:0.4mL/min; 进样量:10μL;流动相A相为1%(v/v)甲酸水溶液(含5mm/L乙酸铵),流动相B为乙 腈。
所述洗脱程序为梯度洗脱,梯度洗脱程序详见表1。
质谱条件:电喷雾离子源,正离子模式;动态多反应监测模式;毛细管电压4.0kV;离子源温度350℃;去溶剂气流:氮气,10L/min;去溶剂温度325℃;锥孔气流:氮 气,8L/min;碰撞气压0.4MPa。
表1.梯度洗脱程序
时间(min) | A(%) | B(%) | 流速(ml/min) |
0.00 | 100.00 | 0.00 | 0.400 |
0.00 | 99.00 | 1.00 | 0.400 |
3.00 | 70.00 | 30.00 | 0.400 |
6.00 | 60.00 | 40.00 | 0.400 |
9.00 | 60.00 | 40.00 | 0.400 |
15.00 | 40.00 | 60.00 | 0.400 |
19.00 | 1.00 | 99.00 | 0.400 |
23.00 | 1.00 | 99.00 | 0.400 |
27.00 | 99.00 | 1.00 | 0.400 |
191种农药为甲胺磷、氧乐果、灭害威、霜霉威、涕灭威亚砜、地虫硫磷、杀线威、 多菌灵、久效磷、氧倍硫磷、灭草烟、百治磷、蚜灭磷、甲硫威亚砜、非草隆、氧倍硫磷 亚砜、N-去甲基啶虫脒、丁咪酰胺、二甲嘧酚、吡虫啉、乙嘧酚、涕灭砜威、二氧威、啶 虫脒、乐果、速灭磷、氧倍硫磷砜、氧化萎锈灵、丁噻隆、甲氧隆、双酰草胺、涕灭威、 胺唑草酮、苯线磷亚砜、环嗪酮、硫环磷、西玛津、速灭威、甲硫威砜、噻吩磺隆、扑灭 通、甲基硫菌灵、特丁通、苯线磷砜、残杀威、马拉氧磷、噁虫威、甲基苯噻隆、倍硫磷 亚砜、绿麦隆、砜拌磷、莠灭净、粉唑醇、环莠隆、甲氧丙净、避蚊胺、甲呋酰胺、氟草 隆、甲霜灵、异丙隆、磺草唑胺、双苯基脲、庚烯磷、对氧磷、异丙威、内吸磷、吡唑草 胺、二甲草胺、双苯酰草胺、异噁草酮、倍硫磷砜、扑灭津、噁唑隆、烯酰吗啉、苄嘧磺 隆、啶斑肟、倍硫磷、甲硫威、扑草净、多效唑、苯锈啶、丁苯吗啉、苯噻菌胺、螺环菌 胺、呋嘧醇、呋菌胺、环丙唑醇、呋霜灵、巴毒磷、灭菌唑、二甲吩草胺、呋草酮、螺虫 乙酯、苯线磷、腈菌唑、咪唑菌酮、苯嘧磺草胺、苯噻酰草胺、异戊乙净、灭线磷、嘧菌 酯、丙溴磷、氟环唑、三唑酮、抑芽唑、草达津、异丙净、嘧菌胺、敌草胺、氟吡菌胺、 氟吡菌酰胺、异噁酰草胺、灭锈胺、稻瘟灵、异丙甲草胺、牧草胺、双炔酰菌胺、氟硅唑、马拉硫磷、乙草胺、戊菌唑、异稻瘟净、乙嘧酚磺酸酯、三唑磷、联苯三唑醇、苯硫威、 氟酰胺、苯氧威、氟噻草胺、拌种胺、醚菌胺、糠菌唑、咪鲜胺、乙基杀扑磷、丙环唑、 敌瘟磷、氟嘧菌酯、甲氧虫酰肼、庚酰草胺、嗪草酸甲酯、溴丁酰草胺、苯霜灵、喹硫磷、 虫酰肼、稻瘟酰胺、多杀霉素、氟丙嘧草酯、异丙草胺、4-十二烷基-2,6-二甲基吗啉、啶 氧菌酯、苯醚甲环唑、磷酸三丁酯、莎稗磷、磷酸三苯酯、二嗪磷、氟菌唑、麦草氟异丙 酯、甲基异柳磷、吡菌磷、禾草丹、吡唑醚菌酯、吡唑解草酯、戊菌隆、特草灵、丙草胺、 哌草磷、苯菌酮、乙基多杀菌素、环氟菌胺、噁唑禾草灵、喹氧灵、肟菌酯、增效醚、甲 氨基阿维菌素、戊草丹、烯禾啶、呋线威、丙硫克百威、噻嗪酮、丁草胺、吡丙醚、吡氟 禾草灵、三甲苯草酮、丁基嘧啶磷、噻螨酮、嘧啶磷、乙螨唑、异噁唑草酮、仲丁灵、唑 螨酯和螺螨酯。
所述净化剂优选乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合硅胶(C18)、石墨化无孔 碳(ENVI-Carb)和碳十八键合锆胶(Z-Sep+)组合使用,乙二胺-N-丙基硅烷(PSA):十八烷基硅 烷键合硅胶(C18):石墨化无孔碳(ENVI-Carb):碳十八键合锆胶 (Z-Sep+)=0.8-1.2:1.8-2.2:0.8-1.2:0.3-0.8,优选乙二胺-N-丙基硅烷(PSA):十八烷基硅烷键合硅胶(C18):石墨化无孔碳(ENVI-Carb):碳十八键合锆胶(Z-Sep+)=1:2:1:0.5;或优选乙二胺-N- 丙基硅烷(PSA)、弗罗里硅土(Florisil)和碳十八键合锆胶(Z-Sep+)组合使用,乙二胺-N-丙基 硅烷(PSA):弗罗里硅土(Florisil):碳十八键合锆胶(Z-Sep+)=0.8-1.2:0.8-1.2:0.8-1.2,优选乙 二胺-N-丙基硅烷(PSA):弗罗里硅土(Florisil):碳十八键合锆胶(Z-Sep+)=1:1:1;或优选十八 烷基硅烷键合硅胶(C18)和多壁碳纳米(Cleaner NANO-carb)组合使用,十八烷基硅烷键合硅 胶(C18):多壁碳纳米(Cleaner NANO-carb)=3.8-4.2:0.8-1.2,优选十八烷基硅烷键合硅胶 (C18):多壁碳纳米(Cleaner NANO-carb)=4:1。
在高油复杂基质样品前处理过程中,为了提高对各类样品的适用范围,有效的降低基 质干扰,在提取时加入萃取溶剂、萃取盐和均质子,净化时加入净化剂,实现目标农药和 基质的有效分离,从而减小高油复杂基质样品的基质干扰,提高检测结果的准确性。极性 溶剂乙腈有较高的提取效率,尤其适用于多残留分析。萃取盐中无水硫酸镁可以有效去除 样品提取时的水分,氯化钠可以起到盐析作用,而乙酸钠、柠檬酸钠、柠檬酸氢二钠可以形成一种酸性的缓冲体系,其一种或多种缓冲盐的使用,有助于农药的提取。均质子的加入,可以通过其产生的剪切力,防止硫酸镁结块并进一步增大高油复杂基质样品与提取液的接触面积,提高提取效率。净化剂的加入可以有效的减少测定过程中同系物、异构体、 降解产物的影响,乙二胺-N-丙基硅烷(PSA)可以有效的去除提取物内的脂肪酸和糖类共萃物;十八烷基硅烷键合硅胶(C18)、二氧化锆胶(Z-Sep)、碳十八键合锆胶(Z-Sep+)、弗罗里硅土(Florisil)和增强型脂质去除剂(EMR-Lipid)可以有效去除体系内的脂类干扰,能够有效 降低提取物中的含油量;石墨化无孔碳(ENVI-Carb)、石墨化碳黑(GCB)和多壁碳纳米(Cleaner NANO-carb)可以有效去除高油复杂基质样品色素所带来的干扰,具有极优的吸附 性。一种或多种净化填料的联用,可以有效的减少高油复杂基质样品的干扰,使前处理的 方法对所有高油复杂基质样品具有普遍适用性。
本发明的有益效果是:
1)本发明提出的一种高油复杂基质样品前处理技术结合UPLC-MSMS测定191种农药残留的方法,通过优化萃取溶剂、萃取盐、净化剂的组合方式,能够提高样品前处理的 通用性,实现对多种高油复杂基质样品的提取净化处理,有效的降低了高油复杂基质样品 农药残留检测过程中所带来的基质干扰,进一步减小了对仪器的损害,有利于降低检测成 本和提高检测人员的熟练程度。
2)本发明提出的前处理方法将样品和提取剂、均质子、萃取盐和净化剂一次性放入 全自动萃取管中,与传统前处理方法相比,避免了多次转移提取液、净化液等步骤所造成 的损失,使用全自动样品制备系统,震荡、离心步骤能在同一个装置中反复进行多次,无需人工转移,能够实现多个样品快速处理,大大节省了样品制备时间,进一步解放了劳动力,对于高油复杂基质样品的提取和净化提供了一种切实可行的方案。
3)本发明提出的一种高油复杂基质样品前处理技术结合UPLC-MSMS测定191种农药残留的方法,能够填补高油复杂基质样品农药多残留的空白,一针进样完成高油复杂基质样品191种农药残留的检测,各农药组分在色谱柱下分离效果好,所测得的检出限、定 量限等各项指标满足农药的多残留分析,可以应用于高油复杂基质样品的多农药残留检测中,对于打破贸易壁垒,促进进出口贸易具有重要意义。
附图说明
图1为191种农药UPLC/MS/MS总离子流图
具体实施方式
实施例1
1材料和方法
1.1材料和试剂
1290高效液相色谱仪和6460三重四极杆质谱仪(美国安捷伦公司);全自动样品制备系统(北京本立科技公司);N-112氮吹浓缩仪(美国Organomation Associates公司),TRIOTM-1N涡旋搅拌器(日本ASONE公司),Milli-Q超纯水机(美国Millipore公司), PL602-L电子天平(瑞士Mettler-Toledo公司),超声波清洗器(中国江苏昆山超声仪器有 限公司)。
191种农药标准品:纯度≥95%(天津阿尔塔公司);乙腈为色谱纯(美国Honeywell公司); 吸附剂:乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合硅胶(C18)吸附剂(天津Bonna-Agela 公司);石墨化无孔碳(ENVI-Carb)、碳十八键合锆胶(Z-Sep+)(美国Supelco公司);甲酸、 乙酸铵(LC-MS级购于Fisher公司);乙酸(分析纯购于北京化工厂);实验用水均为高纯水(经 Milli-Q超纯水器纯化)。
1.2标准溶液的配制
准确称取各标准品(10.0±0.1)mg,分别置于10ml棕色容量瓶中,准确加入10ml甲醇, 配置成1000mg/L的标准储备液,于-18℃冰箱内保存。准确吸取1000mg/L的标准储备液各100ul,置于10ml棕色储备液中,使用甲醇准确定容至10ml,配置为混合标准溶液,于 -4℃冰箱内保存待用。使用甲醇进行梯度稀释,分别稀释为浓度为5mg/L、1mg/L、0.5mg/L、0.4mg/L、0.2mg/L、0.1mg/L的混合标准工作液,于-4℃冰箱内保存待用。
1.3样品前处理
称取粉碎均匀的胡椒2g于离心管外萃取管中,加入高纯水10ml,涡旋1min,静置30min,离心管外萃取管加入15ml 1%乙酸酸化乙腈、12颗陶瓷均质子、6g无水硫酸镁和1.5g乙酸钠,内插管加入500mg无水硫酸镁、6颗陶瓷均质子、200mg乙二胺-N-丙基硅 烷(PSA)、400mg十八烷基硅烷键合硅胶(C18)、200mg石墨化无孔碳(ENVI-Carb)和100mg 碳十八键合锆胶(Z-Sep+),把内插管嵌套入外萃取管中拧好,放入全自动前处理设备,设 置初次振荡10分钟,离心5分钟;二次振荡5分钟,离心5分钟,进行处理。处理结束 后,然后取2ml上清液,40度水浴氮吹至干,加入1ml乙腈:水(3:2)超声复溶,过0.22μm 滤膜,待上机检测。
1.4仪器条件
色谱条件:ZORBAXSB-C18色谱柱,2.1mm×100mm,3.5μm;柱温:40℃;流速: 0.4mL/min;进样量:10μL;流动相:A为1%(v/v)甲酸水溶液(含5mm/L乙酸铵),B 为乙腈;
质谱条件:电喷雾离子源,正离子模式;动态多反应监测模式;毛细管电压4.0kV;离子源温度350℃;去溶剂气流:氮气,10L/min;去溶剂温度325℃;锥孔气流:氮气, 8L/min;碰撞气压0.4MPa。
洗脱程序为梯度洗脱,梯度洗脱程序详见表2。191种农药化合物质谱参数见表3。
表2.梯度洗脱程序
时间(min) | A(%) | B(%) | 流速(ml/min) |
0.00 | 100.00 | 0.00 | 0.400 |
0.00 | 99.00 | 1.00 | 0.400 |
3.00 | 70.00 | 30.00 | 0.400 |
6.00 | 60.00 | 40.00 | 0.400 |
9.00 | 60.00 | 40.00 | 0.400 |
15.00 | 40.00 | 60.00 | 0.400 |
19.00 | 1.00 | 99.00 | 0.400 |
23.00 | 1.00 | 99.00 | 0.400 |
27.00 | 99.00 | 1.00 | 0.400 |
表3 191种农药化合物质谱参数
2方法学验证-标准曲线、检出限、定量限、回收率和精密度的测定
选胡椒阴性样品为空白基质,每种农药选取7个浓度(5、10、20、40、60、80、100 μg/L)制备基质匹配标准溶液,并测定其线性范围,各种农药在其各自线性范围内,呈良 好线性关系,相关系数(R2)>0.995。采用信噪比法测定其检出限与定量限,以信噪比S/N=3 确定方法的检出限(LOD),S/N=10确定方法的定量限(LOQ)。按照实验方法,进行添加回 收实验,选取低(10μg/kg)、中(50μg/kg)、高(100μg/kg)三个浓度为添加回收水平, 每个添加水平进行6组实验,结果表明191种农药其平均回收率范围为70.49-119.02%,相 对标准偏差<13.9%,具体数值见表4。
表4 191种化合物检出限、定量限和线性相关系数及回收率
3结论
本发明实现了自动样品制备与液相色谱三重四极杆串联质谱相结合,建立了高油复杂 基质样品中191种农药残留检测方法,实现了前处理过程的全自动,该方法定量准确,灵 敏度、准确度、精密度和线性关系良好,能够满足市售胡椒、花椒、桂皮、八角等样品中的农药残留检测。
实施例2
采用本发明方法实测市售桂皮20批次,共12批检出农药残留,检出农药17种,其中苯氧威检出农药检出浓度最高为49.3ug/kg,第8批次样品检出农药数量最多为5种,分别检出乙草胺、多效唑、苯霜灵、嘧菌酯和三唑磷。
表5桂皮实测样品农药种类及含量
Claims (10)
1.一种高油复杂基质样品前处理技术结合UPLC-MSMS测定191种农药残留的方法,其特征是,包括以下步骤:
(1)高油复杂基质样品前处理过程:
称取适量样品于离心管外萃取管中,加入超纯水、乙酸酸化乙腈、陶瓷均质子和萃取盐,内插管中加入萃取盐、净化剂和陶瓷均质子,把内插管嵌套入外萃取管中拧好,置于全自动样品处理设备,经反复震荡、多次离心处理后,取内插管中适量上清液,氮吹至近干,加入1ml乙腈:水(3:2)超声复溶,过0.22μm滤膜,待上机检测;
所述萃取盐为:无水硫酸镁和氯化钠、乙酸钠、柠檬酸钠、柠檬酸氢二钠的一种或多种;所述净化剂为乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合硅胶(C18)、石墨化无孔碳(ENVI-Carb)、石墨化碳黑(GCB)、多壁碳纳米(Cleaner NANO-carb)、二氧化锆胶(Z-Sep)、碳十八键合锆胶(Z-Sep+)、弗罗里硅土(Florisil)、增强型脂质去除剂(EMR-Lipid)的一种或多种;
(2)UPLC-MS/MS检测过程:
色谱条件:色谱柱为C18色谱柱,2.1mm×100mm,3.5μm;柱温:40℃;流速:0.4mL/min;进样量:10μL;流动相A相为1%(v/v)甲酸水溶液(含5mm/L乙酸铵),流动相B为乙腈;洗脱程序为梯度洗脱,梯度洗脱程序详见下表:
质谱条件:电喷雾离子源,正离子模式;动态多反应监测模式;毛细管电压4.0kV;离子源温度350℃;去溶剂气流:氮气,10L/min;去溶剂温度325℃;锥孔气流:氮气,8L/min;碰撞气压0.4Mpa;
191种农药为甲胺磷、氧乐果、灭害威、霜霉威、涕灭威亚砜、地虫硫磷、杀线威、多菌灵、久效磷、氧倍硫磷、灭草烟、百治磷、蚜灭磷、甲硫威亚砜、非草隆、氧倍硫磷亚砜、N-去甲基啶虫脒、丁咪酰胺、二甲嘧酚、吡虫啉、乙嘧酚、涕灭砜威、二氧威、啶虫脒、乐果、速灭磷、氧倍硫磷砜、氧化萎锈灵、丁噻隆、甲氧隆、双酰草胺、涕灭威、胺唑草酮、苯线磷亚砜、环嗪酮、硫环磷、西玛津、速灭威、甲硫威砜、噻吩磺隆、扑灭通、甲基硫菌灵、特丁通、苯线磷砜、残杀威、马拉氧磷、噁虫威、甲基苯噻隆、倍硫磷亚砜、绿麦隆、砜拌磷、莠灭净、粉唑醇、环莠隆、甲氧丙净、避蚊胺、甲呋酰胺、氟草隆、甲霜灵、异丙隆、磺草唑胺、双苯基脲、庚烯磷、对氧磷、异丙威、内吸磷、吡唑草胺、二甲草胺、双苯酰草胺、异噁草酮、倍硫磷砜、扑灭津、噁唑隆、烯酰吗啉、苄嘧磺隆、啶斑肟、倍硫磷、甲硫威、扑草净、多效唑、苯锈啶、丁苯吗啉、苯噻菌胺、螺环菌胺、呋嘧醇、呋菌胺、环丙唑醇、呋霜灵、巴毒磷、灭菌唑、二甲吩草胺、呋草酮、螺虫乙酯、苯线磷、腈菌唑、咪唑菌酮、苯嘧磺草胺、苯噻酰草胺、异戊乙净、灭线磷、嘧菌酯、丙溴磷、氟环唑、三唑酮、抑芽唑、草达津、异丙净、嘧菌胺、敌草胺、氟吡菌胺、氟吡菌酰胺、异噁酰草胺、灭锈胺、稻瘟灵、异丙甲草胺、牧草胺、双炔酰菌胺、氟硅唑、马拉硫磷、乙草胺、戊菌唑、异稻瘟净、乙嘧酚磺酸酯、三唑磷、联苯三唑醇、苯硫威、氟酰胺、苯氧威、氟噻草胺、拌种胺、醚菌胺、糠菌唑、咪鲜胺、乙基杀扑磷、丙环唑、敌瘟磷、氟嘧菌酯、甲氧虫酰肼、庚酰草胺、嗪草酸甲酯、溴丁酰草胺、苯霜灵、喹硫磷、虫酰肼、稻瘟酰胺、多杀霉素、氟丙嘧草酯、异丙草胺、4-十二烷基-2,6-二甲基吗啉、啶氧菌酯、苯醚甲环唑、磷酸三丁酯、莎稗磷、磷酸三苯酯、二嗪磷、氟菌唑、麦草氟异丙酯、甲基异柳磷、吡菌磷、禾草丹、吡唑醚菌酯、吡唑解草酯、戊菌隆、特草灵、丙草胺、哌草磷、苯菌酮、乙基多杀菌素、环氟菌胺、噁唑禾草灵、喹氧灵、肟菌酯、增效醚、甲氨基阿维菌素、戊草丹、烯禾啶、呋线威、丙硫克百威、噻嗪酮、丁草胺、吡丙醚、吡氟禾草灵、三甲苯草酮、丁基嘧啶磷、噻螨酮、嘧啶磷、乙螨唑、异噁唑草酮、仲丁灵、唑螨酯和螺螨酯。
2.根据权利要求1所述的方法,其特征在于:所述高油复杂基质样品为花生、花椒、芝麻、八角、桂皮、胡椒、孜然、香叶、陈皮中的一种。
3.根据权利要求1所述的方法,其特征在于:所述外萃取管所加提取剂为1%乙酸酸化乙腈和超纯水,按体积比计,1%乙酸酸化乙腈:超纯水=3:2。
4.根据权利要求1所述的方法,其特征在于:所述萃取盐为无水硫酸镁:乙酸钠=4:1。
5.根据权利要求1所述的方法,其特征在于:所述萃取盐为无水硫酸镁:柠檬酸钠:柠檬酸氢二钠=4:1:1。
6.根据权利要求1所述的方法,其特征在于:所述萃取盐为无水硫酸镁:氯化钠=2:1。
7.根据权利要求1所述的方法,其特征在于:所述净化剂为乙二胺-N-丙基硅烷(PSA):十八烷基硅烷键合硅胶(C18):石墨化无孔碳(ENVI-Carb):碳十八键合锆胶(Z-Sep+)=0.8-1.2:1.8-2.2:0.8-1.2:0.3-0.8,或乙二胺-N-丙基硅烷(PSA):弗罗里硅土(Florisil):碳十八键合锆胶(Z-Sep+)=0.8-1.2:0.8-1.2:0.8-1.2,或十八烷基硅烷键合硅胶(C18):多壁碳纳米(Cleaner NANO-carb)=3.8-4.2:0.8-1.2。
8.根据权利要求1所述的方法,其特征在于:所述净化剂为乙二胺-N-丙基硅烷(PSA):十八烷基硅烷键合硅胶(C18):石墨化无孔碳(ENVI-Carb):碳十八键合锆胶(Z-Sep+)=1:2:1:0.5,或乙二胺-N-丙基硅烷(PSA):弗罗里硅土(Florisil):碳十八键合锆胶(Z-Sep+)=1:1:1,或十八烷基硅烷键合硅胶(C18):多壁碳纳米(Cleaner NANO-carb)=4:1。
9.根据权利要求1所述的方法,其特征在于:全自动样品处理程序为:①振荡频率1100rpm、振荡10分钟;4200rpm、离心5分钟;②振荡频率1100rpm、振荡5分钟;4200rpm、离心5分钟。
10.根据权利要求1所述的方法,其特征在于,高油复杂基质样品、水、1%乙酸酸化乙腈提取液与萃取盐的质量体积比为2g:10ml:15ml:7.5g。
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