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.
本文参考文献
| [1] |
Wegener J W M, Cofino W P, Maier E A, et al. The Preparation, Testing and Certification of Two Freshwater Sediment Reference Materials for Polycyclic Aromatic Hydrocarbons and Polychlorinated Biphenyls: BCR CRM 535 and CRM 536[J].Trends in Analytical Chemistry, 1999, 18(1): 14-25. doi: 10.1016/S0165-9936(98)00087-9 |
| [2] |
de Voogt P, Maier E A, Kramer G N, et al. The Certification of the Contents (Mass Fraction) of Pyrene, Benz[a]anthracene, Benzo[a]pyrene, Benzo[e]pyrene, Benzo[b]fluoranthene, Benzo[k]fluoranthene, Indeno[1, 2, 3-cd]pyrene, Benzo[b]naphtha[2, 1-d]thiophene and Pentachlorophenol in Dried Contaminated Industrial Soil CRM 524, EUR 16933 EN[R]. Brussels: Commission of the European Communities, Community Bureau of Reference, 1996. |
| [3] |
Schantz M M, Jr Benner B A, Hays M J, et al. Certification of Standard Reference Material (SRM)1941a, Organics in Marine Sediment[J].Fresenius' Journal of Analytical Chemistry, 1995, 352: 166-173. doi: 10.1007/BF00322319 |
| [4] |
Wise S A, Schantz M M, Benner B A, et al. Certification of Polycyclic Aromatic Hydrocarbons in a Marine Sediment Standard Reference Material[J].Analytical Chemistry, 1995, 67: 1171-1178. doi: 10.1021/ac00103a006 |
| [5] |
Wise S A, Poster D L, Schantz M M, et al. Two New Marine Sediment Standard Reference Materials(SRMs) for the Determination of Organic-contaminants[J].Analytical and Bioanalytical Chemistry, 2004, 378: 1251-1264. doi: 10.1007/s00216-003-2431-y |
| [6] |
Itoh N, Aoyagi Y, Takatsu A, et al. Certified reference Material for Quantification of Polycyclic Aromatic Hydrocarbons in Sediment from the National Metrology Institute of Japan[J].Analytical and Bioanalytical Chemistry, 2009, 393: 2039-2049. doi: 10.1007/s00216-009-2675-2 |
| [7] |
Yarita T, Takatsu A, Inagaki K, et al. Matrix Certified Reference Materials for Environmental Monitoring from the National Metrology Institute of Japan (NMIJ)[J].Accreditation and Quality Assurance, 2007, 12: 156-160. doi: 10.1007/s00769-006-0204-y |
| [8] |
LGC 6188. Statement of Measurement. River Sediment-PAHs[R]. LGC, 2000. |
| [9] |
高丽荣, 郑明辉, 李敬光, 等. 土壤中多氯联苯成分分析标准物质的研制与定值[J]. 分析化学, 2006, 34(11): 1579-1582. doi: 10.3321/j.issn:0253-3820.2006.11.014 Gao L R, Zheng M H, Li J G, et al. Preparation, Testing and Certification of Soil Reference Materials for Polychlorinated Biphenyls[J].Chinese Journal of Analytical Chemistry, 2006, 34(11): 1579-1582. doi: 10.3321/j.issn:0253-3820.2006.11.014 |
| [10] |
全国标准物质管理委员会. 标准物质的研制管理与应用[M] . 北京: 中国计量出版社, 2010 National Administrative Committee for Certified Reference Material . Preparation, Management and Application of Reference Material[M] . Beijing: China Metrology Publishing House, 2010 |
| [11] |
徐锐锋, 方向, 徐蓓, 等. 同位素稀释质谱法在痕量有机物测量国际比对中的应用[J]. 质谱学报, 2000, 21(3-4): 167-168. Xu R F, Fang X, Xu B, et al. Applications of Isotope Dilution Mass Spectrometry in International Comparisons[J]. Journal of Chinese Mass Spectrometry Society, 2000, 21(3-4): 167-168. |
| [12] |
卢宪波, 陈吉平, 王淑秋, 等. 贻贝中有机氯农药和多氯联苯标准物质的研制及同位素稀释高分辨质谱法定值[J]. 色谱, 2012, 30(9): 915-921. Lu X B, Chen J P, Wang S Q, et al. Preparation and Certification of Mussel Reference Material for Organochlorine Pesticides and Polychlorinated Biphenyls Using Isotope Dilution-High Resolution Mass Spectrometry[J]. Chinese Journal of Chromatography, 2012, 30(9): 915-921. |
| [13] |
全国标准物质管理委员会. 标准物质的研制管理与应用[M] . 北京: 中国质检出版社, 2011 National Administrative Committee for Certified Reference Material . Reference Material-General and Statistical Principles for Certification[M] . Beijing: China Zhijian Publishing House, 2011 |
引证文献（本文共被引用5次）
| [1] |
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) |
| [2] |
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) |
| [3] |
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) |
| [4] |
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) |
| [5] |
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 |
相似文献（共20条）
| [1] |
黄园英, 吴淑琪, 佟玲, 张玲金. 土壤中持久性有机污染物分析的前处理方法. 岩矿测试, 2008, 27(2): 81-86. |
| [2] |
孙玮琳, 沈斌, 汪双清, 龚迎莉. 自然水体和土壤中氯代烃和芳香烃类化合物分析测试方法研究. 岩矿测试, 2008, 27(3): 174-178. |
| [3] |
饶竹, 何淼. 圆盘固相萃取富集-气相色谱法测定地表水中有机氯和有机磷农药. 岩矿测试, 2008, 27(1): 12-16. |
| [4] |
刘广民, 尹莉莉, 董永亮, 肖宇芳. 土壤中五氯酚的快速测定. 岩矿测试, 2008, 27(2): 117-119. |
| [5] |
魏峰, 沈小明, 陈海英, 沈加林. 土壤和沉积物中22种有机氯农药和8种多氯联苯的气相色谱分析. 岩矿测试, 2013, 32(6): 952-958. |
| [6] |
佟 玲, 吴淑琪, 杨佳佳, 张玲金. 土壤中25种有机氯农药和多氯联苯的气相色谱分析方法研究. 岩矿测试, 2010, 29(3): 277-281. |
| [7] |
张岩, 张景发, 陈艳梅, 孟娟, 韩翠英. 加速溶剂萃取-气相色谱法测定土壤中有机氯农药和多氯联苯. 岩矿测试, 2010, 29(5): 491-496. |
| [8] |
陈卫明, 李庆霞, 张芳, 何小辉, 张勤. 加速溶剂萃取-气相色谱/气相色谱-质谱法测定土壤中7种多氯联苯. 岩矿测试, 2011, 30(1): 33-39. |
| [9] |
方金梅. 福州市土壤硒形态分析及其迁移富集规律. 岩矿测试, 2008, 27(2): 103-107. |
| [10] |
佟玲, 杨佳佳, 阎妮, 吴淑琪. 加速溶剂提取/GC-MS同时测定动物组织中有机氯农药和多氯联苯. 岩矿测试, 2014, 33(2): 262-269. |
| [11] |
曹孝文, 邹宽, 徐丹, 沈伟健, 练鸿振, 葛欣, 沈崇钰. 食品中有机氯农药和多氯联苯气相色谱-质谱分析的离子化方式. 岩矿测试, 2013, 32(1): 22-27. |
| [12] | |
| [13] |
薛源, 杨永亮, 万奎元, 吴学丽, 朱晓华, 王晓春, 罗松光. 沈阳市细河周边农田土壤和大气中有机氯农药和多氯联苯初步研究. 岩矿测试, 2011, 30(1): 27-32. |
| [14] |
齐璐璐, 赵会芹, 陈子学, 郑育锁, 孟凡辉, 肖波, 张颖. 连续光源原子吸收光谱法测定土壤水溶性盐中钙镁. 岩矿测试, 2008, 27(2): 95-98. |
| [15] |
马晗宇, 刘菲, 刘玉龙. 气相色谱法测定地下水中有机氯农药和多氯联苯. 岩矿测试, 2010, 29(5): 527-530. |
| [16] |
杨佳佳, 佟玲, 吴淑琪, 阎妮. 加速溶剂萃取-气相色谱法测定谷物中有机氯农药和多氯联苯. 岩矿测试, 2013, 32(3): 487-494. |
| [17] |
武振艳, 杨永亮, 安丽华, 焦杏春, 路国慧, 刘晓端, 徐 清, 谢文明. 新江湾城开发区表层土壤中有机氯农药和多氯联苯的分布特征. 岩矿测试, 2010, 29(3): 231-235. |
| [18] |
万奎元, 杨永亮, 薛源, 武振艳, 朱晓华, 吴学丽, 王晓春, 罗松光. 长白山表层土壤中有机氯农药和多氯联苯的海拔高度分布特征. 岩矿测试, 2011, 30(2): 150-154. |
| [19] |
刘清辉, 曹攽, 马军, 李云木子. 气相色谱-质谱法测定水中8种多氯联苯. 岩矿测试, 2010, 29(5): 523-526. |
| [20] |
汪瑾彦, 汤 桦, 陈大舟, 吴 雪, 冯 洁, 吴学丽, 李 蕾. 气相色谱-质谱法同时测定河流沉积物中多环芳烃和有机氯农药. 岩矿测试, 2010, 29(3): 225-230. |
计量
- PDF下载量(959)
- 文章访问量(2976)
- HTML全文浏览量(52)
- 被引次数(5)