中华预防医学杂志
中華預防醫學雜誌
중화예방의학잡지
CHINESE JOURNAL OF
2013年
1期
59-62
,共4页
张燕%钱杰峰%刘兰侠%赵慧琴
張燕%錢傑峰%劉蘭俠%趙慧琴
장연%전걸봉%류란협%조혜금
水%甲醚类%静态顶空%动态顶空%气相色谱
水%甲醚類%靜態頂空%動態頂空%氣相色譜
수%갑미류%정태정공%동태정공%기상색보
Water%Methyl ethers%Static headspace%Dynamic headspace%Gas chromatography
目的 建立并比较水中苯甲醚的静态顶空气相色谱氢火焰检测器的方法(以下称静态顶空法)和吹扫捕集气相色谱质谱的方法(以下称动态顶空法).方法 静态顶空方法为氮气做载气,10 ml水样品加入5 g NaC1做基质改性剂,75℃高速振摇平衡30 min后,用气相色谱测定苯甲醚的含量,采用外标法定量.动态顶空法为氦气做载气,将5.0 ml水样和0.004 mg/L的内标物氟代苯注入吹脱捕集装置中,经吹扫、捕集和脱附后,用气相色谱质谱仪测定,通过苯甲醚的保留时间及质谱图与谱库中的质谱图作对照进行定性.采用内标法进行定量分析,并对两种方法的检出限、精密度、准确度进行评价.结果 测定苯甲醚静态顶空气相色谱法和动态顶空气相色谱质谱法分别在10 ～ 500 μg/L和0.5～ 60.0 μg/L范围内有良好的线性关系；线性方程分别为Y=782.150X+1.3446和Y=0.0358X-0.0209,相关系数均≥0.999;检出限分别为0.002 μg/L和0.110 μg/L;最低定量限分别为0.006 μg/L、0.350 μg/L,RSD分别在1.8％ ～2.3％和2.0％ ～ 3.4％之间,样品加标回收率在93％～ 101％和96％ ～101％之间.结论 静态顶空气相色谱法和动态顶空气相色谱质谱法操作简单,能快速、灵敏、准确地测定水中苯甲醚的含量.
目的 建立併比較水中苯甲醚的靜態頂空氣相色譜氫火燄檢測器的方法(以下稱靜態頂空法)和吹掃捕集氣相色譜質譜的方法(以下稱動態頂空法).方法 靜態頂空方法為氮氣做載氣,10 ml水樣品加入5 g NaC1做基質改性劑,75℃高速振搖平衡30 min後,用氣相色譜測定苯甲醚的含量,採用外標法定量.動態頂空法為氦氣做載氣,將5.0 ml水樣和0.004 mg/L的內標物氟代苯註入吹脫捕集裝置中,經吹掃、捕集和脫附後,用氣相色譜質譜儀測定,通過苯甲醚的保留時間及質譜圖與譜庫中的質譜圖作對照進行定性.採用內標法進行定量分析,併對兩種方法的檢齣限、精密度、準確度進行評價.結果 測定苯甲醚靜態頂空氣相色譜法和動態頂空氣相色譜質譜法分彆在10 ～ 500 μg/L和0.5～ 60.0 μg/L範圍內有良好的線性關繫；線性方程分彆為Y=782.150X+1.3446和Y=0.0358X-0.0209,相關繫數均≥0.999;檢齣限分彆為0.002 μg/L和0.110 μg/L;最低定量限分彆為0.006 μg/L、0.350 μg/L,RSD分彆在1.8％ ～2.3％和2.0％ ～ 3.4％之間,樣品加標迴收率在93％～ 101％和96％ ～101％之間.結論 靜態頂空氣相色譜法和動態頂空氣相色譜質譜法操作簡單,能快速、靈敏、準確地測定水中苯甲醚的含量.
목적 건립병비교수중분갑미적정태정공기상색보경화염검측기적방법(이하칭정태정공법)화취소포집기상색보질보적방법(이하칭동태정공법).방법 정태정공방법위담기주재기,10 ml수양품가입5 g NaC1주기질개성제,75℃고속진요평형30 min후,용기상색보측정분갑미적함량,채용외표법정량.동태정공법위양기주재기,장5.0 ml수양화0.004 mg/L적내표물불대분주입취탈포집장치중,경취소、포집화탈부후,용기상색보질보의측정,통과분갑미적보류시간급질보도여보고중적질보도작대조진행정성.채용내표법진행정량분석,병대량충방법적검출한、정밀도、준학도진행평개.결과 측정분갑미정태정공기상색보법화동태정공기상색보질보법분별재10 ～ 500 μg/L화0.5～ 60.0 μg/L범위내유량호적선성관계；선성방정분별위Y=782.150X+1.3446화Y=0.0358X-0.0209,상관계수균≥0.999;검출한분별위0.002 μg/L화0.110 μg/L;최저정량한분별위0.006 μg/L、0.350 μg/L,RSD분별재1.8％ ～2.3％화2.0％ ～ 3.4％지간,양품가표회수솔재93％～ 101％화96％ ～101％지간.결론 정태정공기상색보법화동태정공기상색보질보법조작간단,능쾌속、령민、준학지측정수중분갑미적함량.
Objective To establish and compare the method of static headspace gas chromatography hydrogen flame detector (static headspace method) and purge and trap gas chromatography-mass spectrometry (dynamic headspace method) of anisole in water.Methods Nitrogen gas was used as carrier gas in the static headspace method,5 g NaC1 as matrix modifier was added into 10 ml water.The sample was balanced with high speed vibration at 75 ℃C for 30 min,and anisole was detected by gas chromatography and quantified with external standard.Helium was used as carrier gas in dynamic headspace method,5.0 ml water and 0.004 mg/L internal standard fluorobenzene was purged into the purge and trap apparatus.After purging,trapping and desorption,anisole was detected by the gas chromatography-mass spectrograph,confirmed by the retention time and comparison of mass-spectrogram in spectrum library and quantified with internal standard.The repeatability and sensitivity of assay were evaluated.Results A good linear range for anisole was observed in static headspace gas chromatography and dynamic headspace gas chromatography-mass spectrometry,within the range of 10-500 μg/L and 0.5-60.0 μg/L respectively.The linear regression equation was Y =782.150X + 1.3446 and Y =0.0358X-0.0209 respectively,both the correlation coefficient ≥ 0.999.The detection limit (LOD) were 0.002 μg/L and O.110 μg/L,the lower limit of quantitation (LOQ) were 0.006 μg/L and 0.350 μg/L,the relative standard deviation(RSD) were 1.8％-2.3％ and 2.0％-3.4％,and the spiking recovery were 93％-101％ and 96％-101％ respectively.Conclusion The methods of static headspace gas chromatography and dynamic headspace gas chromatography-mass spectrometry are simple and can measure anisole in water quickly,sensitively and accurately.
