中国典型类型土壤中有机氯农药和多氯联苯成分分析标准物质的研制
国家地质实验测试中心, 北京 100037 |
Preparation of Certified Reference Materials of Organochlorine Pesticides and Polychlorinated Biphenyls in Chinese Typical Soils
National Research Center for Geoanalysis, Beijing 100037, China |
摘要：目前在我国有1个有机氯农药(OCPs)分析标准物质, 3个多氯联苯(PCBs)分析标准物质; 国际上欧洲有1个OCPs分析标准物质和2个PCBs分析标准物质。美国、国际原子能机构和日本等组织研制了沉积物中OCPs、PCBs和多环芳烃的有机分析标准物质, 这些标准物质的基质性质、浓度水平与我国地质样品基质性质、实际污染情况不符。本文针对我国土壤类型的分布特点、污染特征及实际样品检测情况, 采集典型地区的土壤作为候选物, 利用传统的气相色谱-质谱法、气相色谱-串联质谱法、气相色谱-电子捕获检测器法和新技术方法——同位素稀释质谱法, 严格按照国家一级标准物质技术规范和相关标准研制了6个土壤有机分析标准物质(编号为GBW07469~GBW07474), 基本涵盖了我国典型土壤类型, 包括褐土、水稻土、黄壤土和草甸土; 定值化合物包括全国地质大调查必测的8种OCPs(α-666、β-666、γ-666、δ-666、p, p'-DDE、p, p'-DDD、o, p'-DDT、p, p'-DDT)和选测的7种PCBs(PCB28、52、101、118、153、138、180), 含量范围为3.9 μg/kg~2.31 mg/kg。此批标准物质的基质性质、目标组分的浓度水平和污染特征与实际环境样品具有较好的一致性, 而且目标物种类多, 含量范围宽, 可以满足我国不同地区、不同程度污染的土壤样品中OCPs和PCBs同时测定的质量监控需求。
Preparation of Certified Reference Materials of Organochlorine Pesticides and Polychlorinated Biphenyls in Chinese Typical Soils
ABSTRACT In China, there is only one certified reference material (CRM) of organochlorine pesticide (OCPs) and three CRMs of polychlorinated biphenyls (PCBs) in soil. Internationally, there is one CRM of OCPs and two CRMs of PCBs in soil in Europe. The National Institute of Standards and Technology (NIST) of the USA, the National Metrology Institute of Japan (NMIJ), and the International Atomic Energy Agency (IAEA) have developed sediment CRMs for OCPs, PCBs and polycyclic aromatic hydrocarbons (PAHs). However, the matrix and contamination levels of CRMs of OCPs and PCBs do not match with the actual pollution of soil in China.In this study, according to the distribution of soil types, pollution levels of organic compounds and quality control requirements of soil samples, the typical soils were collected as candidates in China. According to the primary standard material specification, 6 CRMs of OCPs and PCBs in different soil types (GBW07469-GBW07474) have been developed. Based on the results from traditional methods including Gas Chromatography-Electron Capture Detector (GC-ECD), Gas Chromatography-Mass Spectrometry (GC-MS), Gas Chromatography-Tandem Mass Spectrometry (GC-MS/MS) and new techniques of Gas Chromatography-Isotope Dilution Mass Spectrometry (GC-IDMS), Gas Chromatography-Isotope Dilution Tandem-Mass Spectrometry (GC-IDMS-MS), certified values and expanded uncertainty for 8 OCPs and 7 PCBs are given. Meanwhile, a GC-ID-HRMS method was used to determine PCBs in candidate reference materials for comparison and validation. These CRMs cover most Chinese soil types, including cinnamon, paddy, yellow and meadow soil. The certified values of OCPs and PCBs in soils range from 3.9 μg/kg to 2.31 mg/kg. As the soils used for CRMs were collected from the field, the matrix and contamination levels of OCPs and PCBs are consistent with actual soils. The CRMs can be used in the quality control of OCPs and PCBs detection in soils of different pollution levels in different regions.
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引证文献（本文共被引用5次）
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QuEChERS-GC/ECD法分析土壤和沉积物中残留有机氯农药和多氯联苯[J]. 蔡小虎,蔡述伟,时磊,沈小明. 环境监控与预警. 2016(03) |
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矿区污染场地土壤重金属元素分析标准样品的研制[J]. 田衎,杨珺,孙自杰,周裕敏,邢书才,封跃鹏. 岩矿测试. 2017(01) |
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土壤类标准样品的稳定性研究方法探讨[J]. 田衎,周裕敏,邢书才,封跃鹏,杨珺,王尧,邱赫男. 理化检验(化学分册). 2017(02) |
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含13种有机氯农药土壤标准样品的研制[J]. 刘海萍,鲁炳闻,房丽萍,杨刚,田衎,封跃鹏. 化工环保. 2016(01) |
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牛肉中二噁英及其类似物标准物质的研制与应用[D]. 池敏.山西医科大学 2016 |
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