色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
11期
1266-1270
,共5页
双重净化%气相色谱%多氯联苯%残留量%植物油
雙重淨化%氣相色譜%多氯聯苯%殘留量%植物油
쌍중정화%기상색보%다록련분%잔류량%식물유
double clean-up%gas chromatography(GC)%polychlorinated biphenyls(PCBs)%residues%vegetable oils
为了考察食用油中7种指示性多氯联苯（PCBs）的残留情况，建立了食用油中痕量多氯联苯测定的双重净化-气相色谱法。以乙腈提取样品，提取液浓缩至干后用正己烷溶解，经浓硫酸、硅胶分散固相萃取双重净化后进行气相色谱分析，外标法定量。优化的色谱条件为：HP-5石英毛细管柱（30 m×0.32 mm×0.25μm）程序升温分离，流速0.8 mL / min，进样量1.00μL，电子捕获检测器检测。结果表明：在优化的条件下，7种多氯联苯在10~500μg / L范围内线性良好，相关系数大于0.999，不同基质中的检出限（ S / N =3）范围为1.8~8.9μg / kg，定量限（ S / N =10）范围为5.9~29.8μg / kg。在橄榄油、花生油和棕榈油空白样品中添加10、20、100μg / kg 3个水平的7种多氯联苯，其加标回收率范围为71.0％~105.5％，相对标准偏差（ RSD）范围为4.0％~11.3％。该方法具有操作简便、快速、准确的特点，可用于植物油中指示性多氯联苯残留量的日常检测。
為瞭攷察食用油中7種指示性多氯聯苯（PCBs）的殘留情況，建立瞭食用油中痕量多氯聯苯測定的雙重淨化-氣相色譜法。以乙腈提取樣品，提取液濃縮至榦後用正己烷溶解，經濃硫痠、硅膠分散固相萃取雙重淨化後進行氣相色譜分析，外標法定量。優化的色譜條件為：HP-5石英毛細管柱（30 m×0.32 mm×0.25μm）程序升溫分離，流速0.8 mL / min，進樣量1.00μL，電子捕穫檢測器檢測。結果錶明：在優化的條件下，7種多氯聯苯在10~500μg / L範圍內線性良好，相關繫數大于0.999，不同基質中的檢齣限（ S / N =3）範圍為1.8~8.9μg / kg，定量限（ S / N =10）範圍為5.9~29.8μg / kg。在橄欖油、花生油和棕櫚油空白樣品中添加10、20、100μg / kg 3箇水平的7種多氯聯苯，其加標迴收率範圍為71.0％~105.5％，相對標準偏差（ RSD）範圍為4.0％~11.3％。該方法具有操作簡便、快速、準確的特點，可用于植物油中指示性多氯聯苯殘留量的日常檢測。
위료고찰식용유중7충지시성다록련분（PCBs）적잔류정황，건립료식용유중흔량다록련분측정적쌍중정화-기상색보법。이을정제취양품，제취액농축지간후용정기완용해，경농류산、규효분산고상췌취쌍중정화후진행기상색보분석，외표법정량。우화적색보조건위：HP-5석영모세관주（30 m×0.32 mm×0.25μm）정서승온분리，류속0.8 mL / min，진양량1.00μL，전자포획검측기검측。결과표명：재우화적조건하，7충다록련분재10~500μg / L범위내선성량호，상관계수대우0.999，불동기질중적검출한（ S / N =3）범위위1.8~8.9μg / kg，정량한（ S / N =10）범위위5.9~29.8μg / kg。재감람유、화생유화종려유공백양품중첨가10、20、100μg / kg 3개수평적7충다록련분，기가표회수솔범위위71.0％~105.5％，상대표준편차（ RSD）범위위4.0％~11.3％。해방법구유조작간편、쾌속、준학적특점，가용우식물유중지시성다록련분잔류량적일상검측。
To investigate the residues of seven indicator polychlorinated biphenyls( PCBs)in vegetable oils,a method was established for the determination of trace PCBs in vegetable oils by double clean-up coupled with gas chromatography( GC). After extracted with acetonitrile, the sample extract was concentrated to dryness followed by re-dissolving with hexane. And the solution was pretreated by adding concentrated sulfuric acid followed cleaned-up with silica gel in dispersive solid-phase extraction protocol,then analyzed by GC with external standard meth-od. Under the optimized chromatographic conditions,the analysis was carried out with a capil-lary column(HP-5,30 m×0. 32 mm×0. 25 μm)at a flow rate of 0. 8 mL / min,and the sample volume was 1. 00 μL. Monitoring with an electron-capture detector,all the target analytes were separated by temperature-programming of the column. Good linearities were obtained in the range of 10-500 μg / L for the seven indicator PCBs with the correlation coefficients greater than 0. 999. For different matrices,the limits of detection(S / N = 3)and limits of quantitation(S / N= 10)were in the range of 1. 8-8. 9 μg / kg and 5. 9-29. 8 μg / kg,respectively. At three spiked levels of 10,20 and 100 μg / kg of the seven indicator PCBs in olive oil,palm oil and peanut oil blank samples,the average recoveries ranged from 71. 0% to 105. 5% with the RSDs of 4. 0% -11. 3% . The method is simple,rapid and accurate,and can be used for the routine analysis of the indicator PCBs in vegetable oils.
