食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2015年
6期
2342-2351
,共10页
王瑶%宋焕禄%周艳%杨辉%林锦%陈旭辉
王瑤%宋煥祿%週豔%楊輝%林錦%陳旭輝
왕요%송환록%주염%양휘%림금%진욱휘
饮用水%挥发性有机物%固相微萃取%气相色谱-质谱联用法
飲用水%揮髮性有機物%固相微萃取%氣相色譜-質譜聯用法
음용수%휘발성유궤물%고상미췌취%기상색보-질보련용법
drinking water%volatile organic compounds%solid phase micro-extraction%gas chromatography-mass spectrometry
目的:通过优化固相微萃取(SPME)条件,确定最优实验条件,建立一种固相微萃取与气相色谱-质谱(GC-MS)联用法测定饮用水中32种挥发性有机物的方法。方法采用固相微萃取-气相色谱-质谱联用法对饮用水中的32种挥发性有机物进行测定,确定各化合物的定性定量参数,并优化固相微萃取条件,如萃取头类型、加盐量、平衡时间、萃取时间、萃取温度等,获得最优的测定条件。结果确定的最优条件为:萃取头:CAR/PDMS萃取头;加盐量:10%;平衡时间:20 min;萃取时间:30 min;萃取温度:60℃。本方法的检出限为0.005~5μg/L,在所测浓度范围内回归曲线的线性相关性良好,加标回收率为74.5%~129.5%, RSD 均不大于15%(n=6)。结论该方法的前处理操作简单,具有较好的精密度和准确度,且检出限远低于国家限定标准,可对饮用水中多种挥发性有机物同时进行分析。
目的:通過優化固相微萃取(SPME)條件,確定最優實驗條件,建立一種固相微萃取與氣相色譜-質譜(GC-MS)聯用法測定飲用水中32種揮髮性有機物的方法。方法採用固相微萃取-氣相色譜-質譜聯用法對飲用水中的32種揮髮性有機物進行測定,確定各化閤物的定性定量參數,併優化固相微萃取條件,如萃取頭類型、加鹽量、平衡時間、萃取時間、萃取溫度等,穫得最優的測定條件。結果確定的最優條件為:萃取頭:CAR/PDMS萃取頭;加鹽量:10%;平衡時間:20 min;萃取時間:30 min;萃取溫度:60℃。本方法的檢齣限為0.005~5μg/L,在所測濃度範圍內迴歸麯線的線性相關性良好,加標迴收率為74.5%~129.5%, RSD 均不大于15%(n=6)。結論該方法的前處理操作簡單,具有較好的精密度和準確度,且檢齣限遠低于國傢限定標準,可對飲用水中多種揮髮性有機物同時進行分析。
목적:통과우화고상미췌취(SPME)조건,학정최우실험조건,건립일충고상미췌취여기상색보-질보(GC-MS)련용법측정음용수중32충휘발성유궤물적방법。방법채용고상미췌취-기상색보-질보련용법대음용수중적32충휘발성유궤물진행측정,학정각화합물적정성정량삼수,병우화고상미췌취조건,여췌취두류형、가염량、평형시간、췌취시간、췌취온도등,획득최우적측정조건。결과학정적최우조건위:췌취두:CAR/PDMS췌취두;가염량:10%;평형시간:20 min;췌취시간:30 min;췌취온도:60℃。본방법적검출한위0.005~5μg/L,재소측농도범위내회귀곡선적선성상관성량호,가표회수솔위74.5%~129.5%, RSD 균불대우15%(n=6)。결론해방법적전처리조작간단,구유교호적정밀도화준학도,차검출한원저우국가한정표준,가대음용수중다충휘발성유궤물동시진행분석。
ABSTRACT:Objective To establish a method for determination of 32 kinds of volatile organic compounds in drinking water using solid phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) based on optimal conditions of SPME. Methods SPME-GS-MS were used on qualitative and quantitative determination of 32 kinds of volatile organic compounds. SPME conditions including SPME coating types, NaCl concentration, incubation time, extraction time and extraction temperature were optimized. Results The optimized conditions were as follows: the best fiber coating was CAR/PDMS;NaCl concentration was 10%;incubation time was 20 min;extraction time was 30 min;and extraction temperature was 60℃. The detection limits of this method fell in the range of 0.005~5 μg/L and there were good linearity relations between the compounds and instrumental responds. RSDs were all no more than 15%(n=6), recovery rates were between 74.5%and 129.5%. Conclusion This method is simple. It has a good precision and accuracy, and its detection limits are far lower than that in the national standards, so it can be applied to the analysis of the volatile organic compounds in drinking water.