分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2014年
10期
1178-1183
,共6页
双重净化%气相色谱法%多氯联苯%残留量%水产品
雙重淨化%氣相色譜法%多氯聯苯%殘留量%水產品
쌍중정화%기상색보법%다록련분%잔류량%수산품
double depuration%gas chromatography( GC)%polychlorinated biphenyls( PCBs)%resi-dues%aquatic products
为考察水产品中7种指示性多氯联苯（ PCBs）残留，建立了水产品中痕量多氯联苯测定的双重净化/气相色谱法。样品用丙酮-正己烷（1：4）混合溶剂提取，提取液经浓硫酸净化后再经硅胶分散固相萃取净化，气相色谱仪分析。优化的色谱条件为：选用HP-5（30 m ×0.32 mm ×0.25μm）石英毛细管柱，流速0.80 mL/min，进样量1.00μL，程序升温分离，采用电子捕获检测器进行测定。结果表明：在优化条件下，7种多氯联苯在10~500μg/kg范围内线性关系良好，相关系数均不低于0.99，不同基质的检出限（ S/N=3）为0.72~4.1μg/kg，定量下限（S/N=10）为2.4~13.7μg/kg。对于鲳鱼、明虾和贻贝的空白样品，在10，20，100μg/kg 3个加标水平下7种多氯联苯的回收率为76.5％~104.8％，相对标准偏差（ RSD）为1.6％~10.4％。本方法操作简便、快速、准确，可用于水产品中指示性多氯联苯残留量的日常检测。
為攷察水產品中7種指示性多氯聯苯（ PCBs）殘留，建立瞭水產品中痕量多氯聯苯測定的雙重淨化/氣相色譜法。樣品用丙酮-正己烷（1：4）混閤溶劑提取，提取液經濃硫痠淨化後再經硅膠分散固相萃取淨化，氣相色譜儀分析。優化的色譜條件為：選用HP-5（30 m ×0.32 mm ×0.25μm）石英毛細管柱，流速0.80 mL/min，進樣量1.00μL，程序升溫分離，採用電子捕穫檢測器進行測定。結果錶明：在優化條件下，7種多氯聯苯在10~500μg/kg範圍內線性關繫良好，相關繫數均不低于0.99，不同基質的檢齣限（ S/N=3）為0.72~4.1μg/kg，定量下限（S/N=10）為2.4~13.7μg/kg。對于鯧魚、明蝦和貽貝的空白樣品，在10，20，100μg/kg 3箇加標水平下7種多氯聯苯的迴收率為76.5％~104.8％，相對標準偏差（ RSD）為1.6％~10.4％。本方法操作簡便、快速、準確，可用于水產品中指示性多氯聯苯殘留量的日常檢測。
위고찰수산품중7충지시성다록련분（ PCBs）잔류，건립료수산품중흔량다록련분측정적쌍중정화/기상색보법。양품용병동-정기완（1：4）혼합용제제취，제취액경농류산정화후재경규효분산고상췌취정화，기상색보의분석。우화적색보조건위：선용HP-5（30 m ×0.32 mm ×0.25μm）석영모세관주，류속0.80 mL/min，진양량1.00μL，정서승온분리，채용전자포획검측기진행측정。결과표명：재우화조건하，7충다록련분재10~500μg/kg범위내선성관계량호，상관계수균불저우0.99，불동기질적검출한（ S/N=3）위0.72~4.1μg/kg，정량하한（S/N=10）위2.4~13.7μg/kg。대우창어、명하화이패적공백양품，재10，20，100μg/kg 3개가표수평하7충다록련분적회수솔위76.5％~104.8％，상대표준편차（ RSD）위1.6％~10.4％。본방법조작간편、쾌속、준학，가용우수산품중지시성다록련분잔류량적일상검측。
To study the residues of seven kinds of indicator polychlorinated biphenyls in aquatic prod-ucts,a method was established for the determination of trace polychlorinated biphenyls in aquatic products by double depuration coupled with gas chromatography( GC). With the mixture of acetone-n-hexane(1 : 4)as extract,the samples were extracted,purified by adding concentrated sulfuric acid followed by clean up with silica gel in dispersive solid-phase extraction protocol,and then ana-lyzed by gas chromatography. Under the optimized chromatographic conditions,the analysis was car-ried out on an HP-5 quartz capillary column(30 m × 0. 32 mm × 0. 25μm)at a flow rate of 0. 80 mL/min,and the sample volume was 1. 00 μL. Monitored with an electron-capture detector,all the tar-get analytes were separated by“temperature-programming ”. Good linearities were obtained in the range of 10-500 μg/kg for seven indicators of polychlorinated biphenyls( PCBs)with correlation co-efficients greater than 0. 99. For different matrices,the limits of detection(S/N=3)and limits of quantitation(S/N=10)were in the ranges of 0. 72-4. 1 μg/kg and 2. 4-13. 7 μg/kg,respective-ly. At three spiked levels of 10,20,100μg/kg,the average recoveries of seven indicators of poly-chlorinated biphenyls( PCBS)from butterfish,shrimp and mussel samples ranged from 76. 5% to 104. 8% with RSDs of 1. 6% -10. 4% . The method was simple,rapid and accurate,and could be used for the routine analysis of indicator polychlorinated biphenyls( PCBs)in aquatic products.
