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刻蚀不锈钢丝固相微萃取气相色谱法检测海水中多氯联苯
宋明,赵行行
0
(国家海洋局大连海洋环境监测中心站,辽宁 大连 116015)
摘要:
用氢氟酸刻蚀不锈钢丝制作了固相微萃取(solid-phase microextraction, SPME)纤维,与气相色谱(gas chromatography, GC)联用直接测定了海水水样中的痕量多氯联苯(polychlorinated biphenyls, PCBs),优化了萃取时间、萃取温度、搅拌速率、解吸温度和解吸时间对SPME的萃取效率的影响。本方法的线性范围可达两个数量级,PCB28和PCB52的线性范围是1.0~100.0 ng/L,其他8种PCBs的线性范围是0.5~50.0 ng/L(除PCB198外,r2均在0.99以上),检出限为0.01~0.10 ng/L。单个纤维间及纤维与纤维间的相对标准偏差分别为2.4%~7.2%和4.9%~8.7%。实际海水样品的加标回收率为80.9%~106.0%。微萃取纤维机械强度高、耐海水腐蚀、寿命长、制作成本低,该方法适用于测定海水水样中的痕量PCBs。
关键词:  海洋化学  固相微萃取  多氯联苯  不锈钢丝  海水样品
DOI:10.3969/J.ISSN.2095-4972.2023.01.015
基金项目:国家海洋局北海分局海洋科技项目资助项目(2015B19)
Determination of polychlorinated biphenyls in seawater samples by etched stainless steel wire solid-phase microextraction-gas chromatography
SONG Ming,ZHAO Hanghang
(Dalian Marine Environmental Monitoring Center Station, SOA, Dalian 116015, China)
Abstract:
A novel method was developed for the direct determination of trace polychlorinated biphenyls(PCBs)in seawater samples using a hydrofluoric acid etched stainless steel wire as a fiber of solid-phase microextraction(SPME)coupled with gas chromatography(GC). The parameters influencing the extraction and efficiency, including extraction time, extraction temperature, stirring rate, desorption temperature and desorption time were optimized. The linear range of the method could reach two orders of magnitude with correlation coefficients higher than 0.99 except PCB198. The linear ranges for PCB28 and PCB52 were from 1.0 to 100.0 ng/L, and the linear ranges for 8 other PCBs were from 0.5 to 50.0 ng/L. The limits of detection were in the range of 0.01-0.10 ng/L. The relative standard deviations were 2.4%-7.2% for a single fiber and 4.9%-8.7% for fiber-to-fiber.The recoveries were 80.9%-106.0% for 10 PCBs standard in seawater samples. High mechanical stability, good seawater corrosion resistance, long life time and low cost were some advantages of the etched stainless steel wire fiber. The proposed method was simple, rapid and sensitive, and it was suitable for determining the trace PCBs in seawater samples.
Key words:  marine chemistry  solid-phase microextraction  polychlorinated biphenyls  stainless steel wire  seawater sample

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