CN111380983A - 一种地表水和土壤中高关注类化学品快速筛查方法 - Google Patents
一种地表水和土壤中高关注类化学品快速筛查方法 Download PDFInfo
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- CN111380983A CN111380983A CN202010400895.3A CN202010400895A CN111380983A CN 111380983 A CN111380983 A CN 111380983A CN 202010400895 A CN202010400895 A CN 202010400895A CN 111380983 A CN111380983 A CN 111380983A
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Abstract
本发明建立了一种地表水和土壤中高关注类化学品快速筛查方法,步骤包括筛选高关注类化学品清单、物质分组、质谱条件和色谱条件优化、质谱库构建、高关注类化学品快速筛查。本发明采用超高效液相色谱‑四极杆/静电场轨道阱高分辨质谱快速筛查地表水和土壤中样品,基于精确质量数、保留时间、特征碎片和同位素分布比例,与高关注化学品质谱库搜索匹配,快速定性;可在70 min获得筛查结果,大大缩短了样品的检测和处理时间,提高了检测效率,为高关注化学品风险评估和风险管理提供了技术支撑。
Description
技术领域
本发明属于环境保护领域,涉及化学品分析方法,具体涉及一种地表水和土壤中高关注类化学品快速筛查方法。
背景技术
2001年,欧盟在其面向未来可持续发展的《化学品政策白皮书》中,提出了革新的化学品风险管理体系-“化学品登记、评估、授权管理体系”(REACH),将PBT化学品及其相关类别的“高持久且高生物累积性”化学品(vPvB)、“致癌、致畸和生殖毒性”(CMR)化学品以及“内分泌干扰物质(EDCs)”等高环境和健康风险化学品定义为“高关注类物质”(SVHCs)。REACH法规自2007年公布实施以来,SVHC候选物质清单在不断地更新,至2018年已达到191种。
目前,我国正处于实施“长江三角洲区域一体化发展”国家战略的关键时期,针对长三角沿江沿海地区化工企业集聚、化学品种类繁多、风险高的特点,单组分检测方法耗时、效率低、成本高,分析检测技术缺乏,欧盟或是国际上的一些标准组织只有针对某些单个高度关注物的测试标准,并没有现成的成熟技术参考资料可以遵循。尽管,赛默飞世尔科技实验室已建有农残质谱数据库pQSM(包括642个农药),兽药质谱数据库vQSM(542个化合物),但是,目前还没有针对高关注类化学品的质谱数据库可用于筛查鉴别。因此,本发明利用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱仪建立高关注类化学品快速筛查方法,以期为实际环境中的有毒有害物质的识别提供一种便捷可靠的方法,为我国化学品全过程风险管控提供技术支撑。
发明内容
本发明建立了一种地表水和土壤中高关注类化学品快速筛查方法,采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查地表水和土壤中样品,基于精确质量数、保留时间、特征碎片和同位素分布比例,与高关注化学品质谱库搜索匹配,快速定性,具体步骤如下:
步骤一、筛选高关注类化学品清单
由加州65号、欧盟高关注、美国NTP致癌清单、美国TRI和美国CCA重点控制清单筛选出46种致癌物;22种生殖毒性化学品;4种欧盟高关注化学品;22种烷基酚&内分泌性化学品;2种PBT/vPvB类化学品;97种PPCPs;27种其他类化学品;共220种化学品清单。
步骤二、化学物质分组
通过欧盟高关注类化学品、PBT/vPvB物质、加州65号名录、美国TRI清单比对,生产使用量调查以及化学品危害性查询,筛选出220种高关注类化学品,基于化学物质用途、结构特征、危害性进行分组,确定分为a、b、c、d四组。
a.致癌/生殖毒性/欧盟高关注(72个):4,4’-亚甲基双(N,N-二甲基苯胺)、2-氨基-1-甲基-6-苯基咪唑[4,5-b]吡啶、吡啶、双(2-甲氧基乙基)醚、磷酸三(2-氯乙基)酯、2-氨基蒽醌、邻苯二甲酸二甲氧乙酯、邻苯二甲酸二异戊酯、联大茴香胺、4,4'-二氨基-3,3'-二甲基联苯、6-甲氧基-间甲苯胺、双氯非那胺、氨鲁米特、灭线磷、1-氨基萘、驱蝇啶、次氮基三乙酸、2-氨基芴、7H-二苯并咔唑、丁酰肼、噁草酮、氰草津、甲基托布津、炔苯酰草胺、丁羟基茴香醚、2-氨基-9H-吡啶[2,3-b]吲哚、甲苯二异氰酸酯、亚砜磷、甲苯咪唑、5-氮杂胞嘧啶核苷、敌草隆、金诺芬、颜料橙5、盐酸甲基苄肼、异环磷酰胺、三唑酮、碱性嫩黄、6-丙基-2-硫尿嘧啶、N-亚硝基二乙胺、乙胺嘧啶、秋水仙素、双香豆素、硫双威、N-亚硝基吗啉、甲巯咪唑、N-亚硝基二正丙胺、4-甲基亚硝胺基-1-3-吡啶基-1-丁酮、氟蚁腙、IQ[2-氨基-3-甲基咪唑并(4,5-F)喹啉]、喹禾灵、六甲基磷酰三胺、2-氨基-3,4-二甲基-3H-咪唑并[4,5-f]喹啉、N-甲基乙酰胺、杀鼠灵、邻苯二甲酸二环己酯、邻氨基苯甲酸肉桂酯、2,6-二甲基苯胺、苏丹-1、腈菌唑、2-甲氧基苯胺、4,4’-四甲基二氨二苯酮、2-萘胺、N-亚硝基二正丁胺、对二氨基联苯、N-亚硝基吡咯烷、1,2-二甲氧基-4-(2-丙烯基)苯、分散橙11、4-氯-2-甲基苯胺、2,4-二氨基甲苯、乙烯基硫、邻氨基偶氮甲苯、4-氨基联苯、二甲戊灵。
b.PPCPs组(97个):包括消炎痛、酮洛芬、阿替洛尔、氯霉素、阿奇霉素、尼莫地平、布洛芬、依托泊甙、利巴韦林、克拉屈滨、依曲替酯、米索前列醇、甲地孕酮-17-乙酸酯、舒林酸、洛伐他汀、克拉霉素、克拉屈滨、更昔洛韦、氨基蝶呤、乙硫异烟胺、米索前列醇、磺胺氯哒嗪、磺胺嘧啶、磺胺甲嘧啶、阿莫沙平、美法仑、替尼泊苷、醋酸甲羟孕酮、丙酸氯倍他索、阿斯巴甜、二氟尼柳、扑米酮、更昔洛韦、甲基托布津、异维A酸、灰黄霉素、匹莫齐特、硝苯地平、金诺芬、脱氢红霉素A、仲丁通、安赛蜜、2-氨基-9H-吡啶[2,3-b]吲哚、5-氮杂胞嘧啶核苷、氟哌啶醇、磺胺二甲嘧啶、硫唑嘌呤、氧氟沙星、诺氟沙星、甲氧苄氨嘧啶、罗红霉素、磺胺吡啶、磺胺二甲氧嗪、苯妥英、萘普生、氟苯尼考、磺胺对甲氧嘧啶、磺胺间甲氧嘧啶、利福昔明、甲硝哒唑、盐酸米诺环素、磺胺甲恶唑、磺胺噻唑、磺胺索嘧啶、磺胺邻二甲氧嘧啶、磺胺甲噻二唑苯甲酰磺胺、地美环素盐酸盐、吐纳麝香、异佛尔酮、环丙沙星、三氯卡班、卤贝他索丙酸酯、利血平、磺胺甲氧哒嗪、吉非罗齐、苯扎贝特、菲诺洛芬、安宫黄体酮、氟哌啶醇、吲哚美辛、磺胺脒、磺胺醋酰、三氯生、氯贝酸、苯达松、水杨酸、奥美普林、依托度酸、卡马西平、黄体酮、雌激素酮、睾酮、己烯雌酚、α-雌二醇、β-雌二醇、雌酮、雌三醇。
c.烷基酚类/EDCs(22个):双酚A、双酚B、双酚AF、双酚S、双酚AP、双酚Z、壬基酚、4-(叔辛基)苯酚、甲基丁香酚、4-叔戊基苯酚、辛基苯酚、3.4-二氯苯酚、2-氨基-4-溴苯酚、4-仲丁基-2,6-二叔丁基苯酚、4-庚基苯酚、4-硝基酚、4-溴-2-氟苯酚、4-溴苯酚、对硝基苯酚、2,4-二叔戊基苯酚、邻氨基苯酚、双氯酚/联苯-2-酚。
d.其他(28个):8-氯茶碱、安赛蜜、偶氮苯、二苯甲酮、二苯胺、对氨基偶氮苯、染料木素、蒽、磷酸三苯酯、磷酸三丁酯、水胺硫磷、2,4-二硝基苯胺、甲草胺、避蚊胺、对苯二胺、3-甲基苯胺、3,4-二氯苯胺、螺内酯、呋喃唑酮、对异丙基苯胺、1,3-二氯苯、2-氯-4-硝基苯胺、嗪草酮、氮烯唑胺、2,4-滴、枯莠隆等、2-(二乙基氨基)乙基1-(间甲苯基)环戊烷-1-羧酸酯、乙烯基硫脲。
分组后分别配制混合标准储备液:
I.配制单标准储备液(20mg/L):准备称取220种高关注类化学品0.01g,用甲醇溶解定容于10mL容量瓶中,配成质量浓度为1000mg/L的标准储备液;分别取200μL(1000mg/L)标准储备液于10mL容量瓶中,用甲醇稀释至刻度,配制质量浓度为20mg/L的标准储备液,储存于4℃冰箱中;
II.配制混合标准储备液(200μg/L):准确吸取100μL各单标准储备液(20mg/L)于10mL容量瓶中,用甲醇稀释至刻度,分别配制a、b、c、d四组质量浓度为200μg/L的混合标准储备液,于4℃下保存。
步骤三、质谱条件和液相色谱条件优化
质谱条件(鞘气、辅助气、喷雾电压、毛细管温度、分辨率、自动增益控制、最大离子注入时间、循环次数、碰撞能量、SIM、Full Scan采集模式)的优化;液相色谱条件(C18、T3色谱柱、流动相缓冲盐、添加浓度)的优化;结合不同化学物质加合离子模式分析,探讨不同类别特征污染物在质谱下的碎裂行为。
色谱条件为:Poroshell 120,EC-C18,150mm×2.1×2.7μm色谱柱,柱温40℃;正离子模式:流动相A为0.1%甲酸,流动相D为乙腈;负离子模式:A为0.05%氨水,流动相D为乙腈。流速为0.3mL/min;进样体积为5μL;流动相梯度为:0min,90%A:10%D;0~2min,90%A:10%D;2~3min,70%A:30%D;3~6min,50%A:50%D;6~9min,40%A:60%D;9~15min,0%A:100%D;15~23min,0%A:100%D;23~23.5min,90%A:10%D;23.5~25min,90%A:10%D。
质谱条件为:电离方式为电喷雾离子源,离子源温度为375℃,离子喷雾电压为3500V,鞘气为40arb,辅助气为10arb,反吹气为0,S-lens RF为50;辅助气压:10arb,喷雾气和碰撞气均为高纯氮气,扫描方式采用数据依赖性扫描(data dependent scan),正离子模式和负离子模式分别进样,此模式包含分辨率为70000的一级全扫描和数据依赖的分辨率为17500的二级扫描,扫描范围为100~1500m/z,一级扫描自动增益控制为1.0e6,离子注入时间为100ms;数据依赖的二级扫描自动增益控制设为1.0e5,最大离子注入时间设为100ms,隔离窗口设为3.0m/z,碰撞能量(NCE)设为30,40,50eV,Loop count设为3,动态排除设为10.0s。
步骤四、质谱库构建
基于数据依赖性扫描(data dependent scan)采集模式,获得目标化合物二级信息,二级信息包括精确质量数、保留时间、结构碎片、同位素分布比例,核对特征碎片后,输入化合物名称、CAS、分子式,形成涵盖化合物母离子精确质量数、保留时间、特征碎片精确质量数、同位素分布比例、极性、碰撞能量、电荷数信息的数据库。
步骤五、高关注类化学品快速筛查
分别建立地表水3种、土壤3种提取方法,适用于220种高关注化学品的非特异性提取方法。
水样提取方法:
A:用盐酸将添加回收水样调节到pH=2,5mL甲醇和5mL水分别活化Oasis HLB固相萃取柱,100mL水样过固相萃取柱,每组三个平行,上样速度为3mL·min-1。上样后,用5mL超纯水淋洗,并在负压条件下抽真空30min使其干燥,5mL甲醇洗脱2次后,用5mL(0.1%氨水)乙腈洗脱,洗脱液经氮吹至干,然后用甲醇定容到1mL,涡旋振荡1min,用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱仪分析。
B:将方法A中的洗脱剂由甲醇:(0.1%氨水)乙腈(1:1)改为二氯甲烷,其他步骤同方法A。方法B可作为方法A的后续补充,对于水样中未有效回收的化学物质做二次洗脱提取。
C:将方法A中的洗脱剂由甲醇:(0.1%氨水)乙腈(1:1)改为甲醇:乙腈(1:1),其他步骤同方法A。方法C也可作为方法A的后续补充,对于水样中未有效回收的化学物质做二次洗脱提取。
土壤样本提取方法:
A(乙腈提取法):取5g土壤样本放入50mL离心管中,加入25mL乙腈,涡旋20s,放入超声清洗机超声15min,提取液,以3mL/min的流速上固相萃取小柱(柱型根据物质种类参考水样提取方法选择),用2mL二氯甲烷淋洗,收集洗脱液,氮吹至干,用乙腈定容至1mL,涡旋振荡1min,过0.22μm滤膜后,待上机分析。
B(甲醇提取法):适提取方法程序:将方法A中的洗脱剂由乙腈改为(1%甲酸)甲醇,其他步骤同方法A。
C(QuEChERs):适提取方法程序:将方法A中的提取液转移至已提前放入150mg PSA和150mg C18吸附剂的离心管中净化,涡旋振荡2min,静置2min,其他步骤同方法A。
前处理后的地表水和土壤样本采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱数据依赖性扫描(data dependent scan)采集模式同步骤三质谱和液相色谱条件进行进样分析。
上样分析后,基于精确质量数、保留时间、特征碎片和同位素分布比例,与高关注类化学品质谱库搜索匹配,采用母离子搜素算法、同位素特征提取算法和结构相似性算法(欧几里得距离法)进行高关注类化学品定性。一级母离子精确质量数质量精度小于百万分之五以内,二级碎片质量精度小于百万分之五,同位素分布误差30%范围内快速筛查出高关注类化学品。
整个分析过程按每10个样品添加1个基质空白、1个样品重复和1个基质加标,平行样品的相对误差小于30%。实验所用锥形瓶、鸡心瓶等玻璃器皿均经丙酮浸泡、烘干,同时避免使用塑料容器。每批样品测定前后,各测定一次标准曲线溶液,用于判断仪器响应变化,其相对变化不大于10%。220种高关注类化学品在5~500μg/L浓度范围内线性良好,相关系数均大于0.9900;回收率达到50.5~119.6%,平行样相对偏差6.9~19.8%;仪器检出限(S/N≥3)为0.008~6.018μg/L,方法的定量限((S/N≥10)为0.027~20.062μg/L。
本发明的有益效果在于:高关注类化学品种类繁多、性质各异、对环境危害大。现有环境检测标准是针对某种或某一类特定物质的靶向分析方法,无法应用于多组分化学品的环境暴露和环境释放水平的监测监控。此外,农残质谱数据库pQSM(包括642个农药),兽药质谱数据库vQSM(542个化合物)也无法快速筛查出未知样本中的高关注类物质。利用本发明一种地表水和土壤中高关注类化学品快速筛查方法,对于高关注类化学品的风险评估和风险管理具有重要意义。实验室不需要购买高关注类化学品标准品情况下,正负离子模式按照本发明仪器方法各进样一次(共50min),与高关注类化学品质谱库匹配定性(20min),在70min内快速鉴定出未知样本中的高关注类化学品。节约了时间,减少了人力、物力、实现了高关注类化学品的准确定性(质量精度在百万分之五以内,保留时间偏差0.2s,二级碎片质量精度小于百万分之五,同位素分布误差30%范围内),本发明建立的高关注化学品快速筛查方法为实际环境中的污染物快速鉴别提供了一种可靠的、可行的方法。
附图说明
图1、物质分组流程图。
图2、质谱条件和色谱条件优化流程图。
图3、高关注类化学品质谱库构建流程图。
图4、高关注类化学品快速筛查流程图。
图5、磷酸三丁酯的同位素分布和特征碎片与高关注类化学品质谱库匹配结果。
具体实施方式
下面结合具体实施例对本发明作进一步详细描述,但并不因此限制本发明的内容。
实施例1
以在重庆涪陵地区水样(W1~W13)和土样(S1~S6)采集的共17个样品进行高关注类化学品快速筛查的为例,采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查,与高关注类化学品质谱库搜索匹配。测定方法包括以下步骤:
步骤一:样品采集:
于2018年7月采集重庆如东洋口化工园区,建峰乌江大桥、潘家坝污水排口、潘家坝污水纳污口、荔枝乌江大桥、涪陵乌江二桥、石板沟长江大桥、涪陵长江大桥、青草背长江大桥、龙桥污水处理厂(纳污水体、排口)、白涛污水处理厂排口设置13个点位(W1~W13),1L于棕色玻璃瓶内,采集13个样品,4℃保存待测。
在蔺市镇、新涪食品有限公司、妙音村、涛达宾馆、建峰浩康厂区和华锋铝业厂区6个点位(S1~S6)采集土壤20g,去除杂物,至于不锈钢盒中,冷冻干燥,研磨过60目筛,-20℃保存待测。
步骤二、样品前处理:
水样提取方法A:用盐酸将添加回收水样调节到pH=2,5mL甲醇和5mL水分别活化Oasis HLB固相萃取柱,100mL水样过柱进行固相萃取,每组三个平行,上样速度为3mL·min-1。上样后,用5mL超纯水淋洗,并在负压条件下抽真空30min使其干燥,5mL甲醇洗脱2次后,用5mL(0.1%氨水)乙腈洗脱,洗脱液经氮吹至干,然后用甲醇定容到1mL,涡旋振荡1min,用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱仪分析。
水样提取方法B:将方法A中的洗脱剂由甲醇:(0.1%氨水)乙腈(1:1)改为二氯甲烷,其他步骤同方法A。方法B可作为方法A的后续补充,对于水样中未有效回收的化学物质做二次洗脱提取。
水样提取方法C:将方法A中的洗脱剂由甲醇:(0.1%氨水)乙腈(1:1)改为甲醇:乙腈(1:1),其他步骤同方法A。方法C也可作为方法A的后续补充,对于水样中未有效回收的化学物质做二次洗脱提取。
土壤样本提取方法A(乙腈提取法):取5g土壤样本放入50mL离心管中,加入25mL乙腈,涡旋20s,放入超声清洗机超声15min,提取液,以3mL/min的流速上固相萃取小柱(柱型根据物质种类参考水样提取方法选择),用2mL二氯甲烷淋洗,收集洗脱液,氮吹至干,用乙腈定容至1mL,涡旋振荡1min,过0.22μm滤膜后,待上机分析。
土壤样本提取方法B(甲醇提取法):适提取方法程序:将方法A中的洗脱剂由乙腈改为(1%甲酸)甲醇,其他步骤同方法A。
土壤样本提取方法C(QuEChERs):适提取方法程序:将方法A中的提取液转移至已提前放入150mg PSA和150mg C18吸附剂的离心管中净化萃取,涡旋振荡2min,静置2min,其他步骤同方法A;
步骤三、超高效液相色谱-四极杆/静电场轨道阱高分辨质谱技术(UHPLC-Q-Exactive MS)进样分析
色谱条件为:Poroshell 120,EC-C18,150mm×2.1×2.7μm色谱柱,柱温40℃;正离子模式:流动相A为0.1%甲酸,流动相D为乙腈;负离子模式:A为0.05%氨水,流动相D为乙腈。流速为0.3mL/min;进样体积为5μL;流动相梯度为:0min,90%A:10%D;0~2min,90%A:10%D;2~3min,70%A:30%D;3~6min,50%A:50%D;6~9min,40%A:60%D;9~15min,0%A:100%D;15~23min,0%A:100%D;23~23.5min,90%A:10%D;23.5~25min,90%A:10%D。
质谱条件为:电离方式为电喷雾离子源,离子源温度为375℃,离子喷雾电压为3500V,鞘气流速为40arb,辅助气为10arb,反吹气为0,S-lens RF为50;辅助气压:10arb,喷雾气和碰撞气均为高纯氮气,扫描方式采用data dependent scan,正离子模式和负离子模式分别进样,此模式包含分辨率为70000的一级全扫描和数据依赖的分辨率为17500的二级扫描,扫描范围为100~1500m/z,一级扫描自动增益控制为1.0e6,离子注入时间为100ms;数据依赖的二级扫描自动增益控制设为1.0e5,最大离子注入时间设为100ms,隔离窗口设为3.0m/z,碰撞能量(NCE)设为30,40,50eV,Loop count设为3,动态排除设为10.0s。
步骤四、高关注类化学品快速筛查
采用赛默飞Trance Finder 4.0软件进行快速定性筛查。由本发明构建的高关注类化学品质谱库,根据母离子搜素算法、同位素特征提取算法和结构相似性算法,基于精确质量数、保留时间、离子碎片和同位素分布比例,在一级母离子精确质量数质量精度小于百万分之五,二级碎片质量精度小于百万分之五,同位素分布误差小于30%进行搜索匹配。其中,水样W1和W9中磷酸三丁酯与高关注类化学品质谱库中磷酸三丁酯精确质量数精度百万分之二,保留时间偏差0.1s以内,同位素分布100%匹配,特征碎片211.1093、155.04677和98.98417,100%匹配;因此W1和W9水样中含有磷酸三丁酯化合物如图5所示。与高关注类化学品质谱库搜索匹配,重庆地表水中快速筛查出52种,土壤中38种,共60种高关注类化学品。
进一步地定量确认:配制86种高关注化学品的混合标准储备液(200μg/L):准确吸取100μL各单标准储备液(20mg/L)于10mL容量瓶中,用甲醇稀释至刻度,配制质量浓度为200μg/L的混合标准储备液,于4℃下保存。
进一步地用甲醇作为溶剂,将上述混合标准储备液(200μg/L)按比例稀释后配成质量浓度分别为1、2、5、10、20、50、100μg/L的混合标准溶液于,44℃下保存。
进一步地绘制标准曲线:用甲醇配制质量浓度分别为1、2、5、10、20、50、100μg/L的混合标准溶液,以峰面积(y)对目标物的质量浓度(x)绘制标准曲线,外标法定量,结果如表2所示。
实施例2
以在三峡地区水样(W1~W22)采集的共22个样品进行高关注类化学品快速筛查的为例,采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查样品,与高关注类化学品质谱库搜索匹配。测定方法包括以下步骤:
步骤一:样品采集
于2019年7月采集三峡沌口、洪湖新滩口、洪湖螺山镇、城陵矶、石首绣林镇、观音寺、陈家店、葛洲坝、太平溪、九畹溪、青干河、香溪河、巴东官渡口、曲尺滩、巫山长江大桥、奉节县长江大桥、磨刀溪、大周、忠州镇顺溪场、凤城镇黄草峡、小溪天生桥、嘉陵江共22个点位(W1~W22),1L于棕色玻璃瓶内,采集22个样品,4℃保存待测。
步骤二、样品前处理
水样提取方法A:用盐酸将添加回收水样调节到pH=2,5mL甲醇和5mL水分别活化Oasis HLB固相萃取柱,100mL水样过柱进行固相萃取,每组三个平行,上样速度为3mL·min-1。上样后,用5mL超纯水淋洗,并在负压条件下抽真空30min使其干燥,5mL甲醇洗脱2次后,用5mL(0.1%氨水)乙腈洗脱,洗脱液经氮吹至干,然后用甲醇定容到1mL,涡旋振荡1min,用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱仪分析。
水样提取方法B:将方法A中的洗脱剂由甲醇:(0.1%氨水)乙腈(1:1)改为二氯甲烷,其他步骤同方法A。方法B可作为方法A的后续补充,对于水样中未有效回收的化学物质做二次洗脱提取。
水样提取方法C:将方法A中的洗脱剂由甲醇:(0.1%氨水)乙腈(1:1)改为甲醇:乙腈(1:1),其他步骤同方法A。方法C也可作为方法A的后续补充,对于水样中未有效回收的化学物质做二次洗脱提取。
步骤三、超高效液相色谱-四极杆/静电场轨道阱高分辨质谱技术(UHPLC-Q-Exactive MS)进样分析
色谱条件为:Poroshell 120,EC-C18,150mm×2.1×2.7μm色谱柱,柱温40℃;正离子模式:流动相A为0.1%甲酸,流动相D为乙腈;负离子模式:A为0.05%氨水,流动相D为乙腈。流速为0.3mL/min;进样体积为5μL;流动相梯度为:0min,90%A:10%D;0~2min,90%A:10%D;2~4min,70%A:30%D;4~6min,50%A:50%D;6~9min,40%A:60%D;9~14min,0%A:100%D;14~16min,90%A:10%D;16~17min,90%A:10%D。
质谱条件为:电离方式为电喷雾离子源,离子源温度为375℃,离子喷雾电压为3500V,鞘气流速为40arb,辅助气为10arb,反吹气为0,S-lens RF为50;辅助气压:10arb,喷雾气和碰撞气均为高纯氮气,扫描方式采用data dependent scan,正离子模式和负离子模式分别进样,此模式包含分辨率为70000的一级全扫描和数据依赖的分辨率为17500的二级扫描,扫描范围为100~1500m/z,一级扫描自动增益控制为1.0e6,离子注入时间为100ms;数据依赖的二级扫描自动增益控制设为1.0e5,最大离子注入时间设为100ms,隔离窗口设为3.0m/z,碰撞能量(NCE)设为30,40,50eV,Loop count设为3,动态排除设为10.0s。
步骤四、高关注类化学品快速筛查
采用赛默飞Trance Finder 4.0软件进行快速定性筛查。由本发明构建的高关注类化学品质谱库,根据母离子搜素算法、同位素特征提取算法和结构相似性算法,基于精确质量数、保留时间、离子碎片和同位素分布匹配,在一级母离子精确质量数质量精度小于百万分之五,二级碎片质量精度小于百万分之五,同位素分布误差小于30%进行搜索匹配,三峡22个地表水样品快速筛查出17个高关注类化学品。
进一步地定量确认:配制31种混合标准储备液(200μg/L):准确吸取100μL各单标准储备液(20mg/L)于10mL容量瓶中,用甲醇稀释至刻度,配制质量浓度为200μg/L的混合标准储备液,于4℃下保存。
进一步地用甲醇作为溶剂,将上述混合标准储备液(200μg/L)按比例稀释后配成质量浓度分别为1、2、5、10、20、50、100μg/L的混合标准溶液于,44℃下保存;
进一步地绘制标准曲线:用甲醇配制质量浓度分别为1、2、5、10、20、50、100μg/L的混合标准溶液,以峰面积(y)对目标物的质量浓度(x)绘制标准曲线,外标法定量,结果如表3所示。
表1 220种高关注类化学品质谱库
表2重庆水样和土壤中确认化学品物质检出浓度(水单位:ng/L;土单位:ng/g)
表3三峡水样确认化学品物质检出浓度(水单位:ng/L)
Claims (8)
1.一种地表水和土壤中高关注类化学品快速筛查方法,其特征在于,所述方法包括以下步骤:
步骤一、筛选高关注类化学品清单;
步骤二、化学物质分组;
步骤三、质谱条件和色谱条件优化;
步骤四、高关注类化学品质谱库构建;
步骤五、地表水和土壤中高关注类化学品快速筛查。
2.根据权利要求1所述的地表水和土壤中高关注类化学品快速筛查方法,其特征在于,所述步骤一为:筛选出46种致癌物;22种生殖毒性化学品;4种欧盟高关注化学品;22种烷基酚和内分泌性化学品;2种PBT/vPvB类化学品;97种PPCPs;27种其他类化学品;共220种化学品清单。
3.根据权利要求2所述的地表水和土壤中高关注类化学品快速筛查方法,其特征在于,所述步骤二为:基于化合物质用途、结构特征、危害性对步骤一化学品进行如下分组:
a.致癌/生殖毒性(72个):4,4’-亚甲基双(N,N-二甲基苯胺)、2-氨基-1-甲基-6-苯基咪唑[4,5-b]吡啶、吡啶、双(2-甲氧基乙基)醚、磷酸三(2-氯乙基)酯、2-氨基蒽醌、邻苯二甲酸二甲氧乙酯、邻苯二甲酸二异戊酯、联大茴香胺、4,4'-二氨基-3,3'-二甲基联苯、6-甲氧基-间甲苯胺、双氯非那胺、氨鲁米特、灭线磷、1-氨基萘、驱蝇啶、次氮基三乙酸、2-氨基芴、7H-二苯并咔唑、丁酰肼、噁草酮、氰草津、甲基托布津、炔苯酰草胺、丁羟基茴香醚、2-氨基-9H-吡啶[2,3-b]吲哚、甲苯二异氰酸酯、亚砜磷、甲苯咪唑、5-氮杂胞嘧啶核苷、敌草隆、金诺芬、颜料橙 5、盐酸甲基苄肼、异环磷酰胺、三唑酮、碱性嫩黄、6-丙基-2-硫尿嘧啶、N-亚硝基二乙胺、乙胺嘧啶、秋水仙素、双香豆素、硫双威、N-亚硝基吗啉、甲巯咪唑、N-亚硝基二正丙胺、4-甲基亚硝胺基-1-3-吡啶基-1-丁酮、氟蚁腙、IQ[2-氨基-3-甲基咪唑并(4,5-F)喹啉]、喹禾灵、六甲基磷酰三胺、2-氨基-3,4-二甲基-3H-咪唑并 [4,5-f]喹啉、N-甲基乙酰胺、杀鼠灵、邻苯二甲酸二环己酯、邻氨基苯甲酸肉桂酯、2,6-二甲基苯胺、苏丹-1、腈菌唑、2-甲氧基苯胺、4,4’-四甲基二氨二苯酮、2-萘胺、N-亚硝基二正丁胺、对二氨基联苯、N-亚硝基吡咯烷、1,2-二甲氧基-4-(2-丙烯基)苯、分散橙11、4-氯-2-甲基苯胺、2,4-二氨基甲苯、乙烯基硫、邻氨基偶氮甲苯、4-氨基联苯、二甲戊灵;
b. PPCPs组(97个):包括消炎痛、酮洛芬、阿替洛尔、氯霉素、阿奇霉素、尼莫地平、布洛芬、依托泊甙、利巴韦林、克拉屈滨、依曲替酯、米索前列醇、甲地孕酮-17-乙酸酯、舒林酸、洛伐他汀、克拉霉素、克拉屈滨、更昔洛韦、氨基蝶呤、乙硫异烟胺、米索前列醇、磺胺氯哒嗪、磺胺嘧啶、磺胺甲嘧啶、阿莫沙平、美法仑、替尼泊苷、醋酸甲羟孕酮、丙酸氯倍他索、阿斯巴甜、二氟尼柳、扑米酮、更昔洛韦、甲基托布津、异维 A 酸、灰黄霉素、匹莫齐特、硝苯地平、金诺芬、脱氢红霉素 A、仲丁通、安赛蜜、2-氨基-9H-吡啶[2,3-b]吲哚、5-氮杂胞嘧啶核苷、氟哌啶醇、磺胺二甲嘧啶、硫唑嘌呤、氧氟沙星、诺氟沙星、甲氧苄氨嘧啶、罗红霉素、磺胺吡啶、磺胺二甲氧嗪、苯妥英、萘普生、氟苯尼考、磺胺对甲氧嘧啶、磺胺间甲氧嘧啶、利福昔明、甲硝哒唑、盐酸米诺环素、磺胺甲恶唑、磺胺噻唑、磺胺索嘧啶、磺胺邻二甲氧嘧啶、磺胺甲噻二唑苯甲酰磺胺、地美环素盐酸盐、吐纳麝香、异佛尔酮、环丙沙星、三氯卡班、卤贝他索丙酸酯、利血平、磺胺甲氧哒嗪、吉非罗齐、苯扎贝特、菲诺洛芬、安宫黄体酮、氟哌啶醇、吲哚美辛、磺胺脒、磺胺醋酰、三氯生、氯贝酸、苯达松、水杨酸、奥美普林、依托度酸、卡马西平、黄体酮、雌激素酮、睾酮、己烯雌酚、α-雌二醇、β-雌二醇、雌酮、雌三醇;
c.烷基酚类(22个):双酚A、双酚B、双酚AF、双酚 S、双酚AP、双酚Z、壬基酚、4-(叔辛基)苯酚、甲基丁香酚、4-叔戊基苯酚、辛基苯酚、3.4-二氯苯酚、2-氨基-4-溴苯酚、4-仲丁基-2,6-二叔丁基苯酚、4-庚基苯酚、4-硝基酚、4-溴-2-氟苯酚、4-溴苯酚、对硝基苯酚、2,4-二叔戊基苯酚、邻氨基苯酚、双氯酚/联苯-2-酚;
d.其他(29个):8-氯茶碱、安赛蜜、偶氮苯、二苯甲酮、二苯胺、对氨基偶氮苯、染料木素、蒽、磷酸三苯酯、磷酸三丁酯、水胺硫磷、2,4-二硝基苯胺、甲草胺、避蚊胺、对苯二胺、3-甲基苯胺、3,4-二氯苯胺、螺内酯、呋喃唑酮、对异丙基苯胺、1,3-二氯苯、2-氯-4-硝基苯胺、嗪草酮、氮烯唑胺、2,4-滴、枯莠隆等、2-(二乙基氨基)乙基 1-(间甲苯基)环戊烷-1-羧酸酯、邻苯二甲酸二丁酯、乙烯基硫脲。
4.根据权利要求1所述的地表水和土壤中高关注类化学品快速筛查方法,其特征在于,步骤三所述的质谱条件包括鞘气、辅助气、喷雾电压、毛细管温度、分辨率、自动增益控制、最大离子注入时间、循环次数、碰撞能量、SIM、Full Scan采集模式;所述色谱条件包括C18、Hillic、T3色谱柱、流动相缓冲盐、添加浓度。
5.根据权利要求4所述的地表水和土壤中高关注类化学品快速筛查方法,其特征在于,优化后的液相色谱条件为:Poroshell 120,EC-C18,150 mm×2.1×2.7µm色谱柱,柱温40℃;正离子模式:流动相A为0.1%甲酸,流动相D为乙腈;负离子模式:A为0.05%氨水,流动相D为乙腈;流速为0.3mL/min;进样体积为5μL;流动相梯度为:0min,90%A:10%D;0~2min,90%A:10%D;2~3min,70%A:30%D;3~6min,50%A:50%D;6~9min,40%A:60%D;9~15min,0%A:100%D;15~23min,0%A:100%D;23~23.5min,90% A:10%D;23.5~25min,90%A:10%D。
6.根据权利要求4所述的地表水和土壤中高关注类化学品快速筛查方法,其特征在于,优化后的质谱条件为:电离方式为电喷雾离子源,离子源温度为375℃,离子喷雾电压为3500V,鞘气为40arb,辅助气为10arb,反吹气为0,S-lens RF为50;辅助气压:10arb,喷雾气和碰撞气均为高纯氮气,扫描方式采用数据依赖性扫描,正离子模式和负离子模式分别进样,此模式包含分辨率为70000的一级全扫描和数据依赖的分辨率为17500的二级扫描,扫描范围为100~1500 m/z,一级扫描自动增益控制为1.0e6,离子注入时间为100 ms;数据依赖的二级扫描自动增益控制设为1.0e5,最大离子注入时间设为100 ms,隔离窗口设为3.0m/z,碰撞能量设为30,40,50eV,循环计数设为3,动态排除设为10.0s。
7.根据权利要求1所述的地表水和土壤中高关注类化学品快速筛查方法,其特征在于,所述步骤四基于数据依赖性扫描,获得目标化合物二级信息,二级信息包括精确质量数、保留时间、结构碎片、同位素分布比例,核对特征碎片后,输入化合物名称、CAS、分子式,形成涵盖化合物母离子精确质量数、保留时间、特征碎片精确质量数、同位素分布比例、极性、碰撞能量、电荷数信息的220种高关注类化学品质谱数据库。
8.根据权利要求1所述的地表水和土壤中高关注类化学品快速筛查方法,其特征在于,所述步骤五具体为:对地表水和土壤样本中的不同类别高关注类化学品进行快速筛查,地表水和土壤样本经以下6种提取方法进行前处理:
水样提取方法A:用盐酸将添加回收水样调节到pH=2,5mL甲醇和5mL水分别活化固相萃取柱,100 mL 水样过固相萃取柱,每组三个平行,上样速度为3 mL∙min-1;上样后,用5 mL超纯水淋洗,并在负压条件下抽真空30 min使其干燥,5mL甲醇洗脱2次后,用含0.1%氨水的5mL乙腈溶液洗脱,洗脱液经氮吹至干,然后用甲醇定容到1 mL,涡旋振荡1 min,用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱仪分析;
水样提取方法B:将方法A中的洗脱剂由甲醇、乙腈溶液改为二氯甲烷,其他步骤同方法A;
水样提取方法C:将方法A中的洗脱剂由甲醇:乙腈溶液改为甲醇:纯乙腈,其他步骤同方法A;
土壤样本提取方法A:取5g土壤样本放入50mL离心管中,加入25mL乙腈,涡旋20 s,放入超声清洗机超声15 min,提取液,以3mL/min的流速上固相萃取小柱,用2 mL二氯甲烷淋洗,收集洗脱液,氮吹至干,用乙腈定容至1mL,涡旋振荡1 min,过0.22μm滤膜后,待上机分析;
土壤样本提取方法B:适提取方法程序:将土壤样本提取方法A中的洗脱剂由乙腈改为含1%甲酸的甲醇溶液,其他步骤同土壤样本提取方法A;
土壤样本提取方法C:适提取方法程序:将土壤样本提取方法A中的提取液转移至已提前放入150 mg PSA和150 mg C18吸附剂的离心管中净化萃取,涡旋振荡2 min,静置2min,其他步骤同土壤样本提取方法A;
按照步骤三色谱、质谱条件进样分析,与高关注类化学品质谱库匹配,采用母离子搜素算法、同位素特征提取算法和结构相似性欧几里得距离法算法进行高关注类化学品匹配,基于精确质量数、保留时间、离子碎片和同位素分布与库里目标物匹配,在一级母离子精确质量数质量精度小于百万分之五,二级碎片质量精度小于百万分之五,同位素分布误差30%范围内筛查高关注类化学品。
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