中华预防医学杂志
中華預防醫學雜誌
중화예방의학잡지
CHINESE JOURNAL OF
2013年
5期
455-458
,共4页
环丙烷类%炭%气相色谱-质谱法%同位素稀释法%饮用水
環丙烷類%炭%氣相色譜-質譜法%同位素稀釋法%飲用水
배병완류%탄%기상색보-질보법%동위소희석법%음용수
Cyclopropanes%Charcoal%Gas-chromatography and mass-spectrometry%Isotope dilution method%Drinking water
目的 建立同位素稀释-气相色谱质谱联用方法测定生活饮用水中环氧氯丙烷.方法 在生活饮用水样品中加入D5-环氧氯丙烷内标应用液,先用活性炭对环氧氯丙烷进行富集,活性炭经2739×g离心脱水10 min,最后加入1.0 ml丙酮浸泡1h并进行解吸,解吸液用气相色谱-质谱法进行测定,同位素内标法定量,并对方法的检测限精密度和准确度进行评价,用该方法对某市25批次饮用水中环氧氯丙烷进行测定.结果 采用该方法测定环氧氯丙烷,在0.0645～3.8700 μg/L范围内线性良好,线性方程为Y=2.828X +4.91×10-2(r＞0.999),测定浓度为0.0806、0.3230、3.2300 μg/L时,环氧氯丙烷的RSD分别为7.9％、4.7％、3.1％；加标平均回收率在95.7％ ～98.7％之间,方法检测限为0.015 μg/L,定量限为0.052 μg/L.检测的25批饮用水中环氧氯丙烷含量均在检测限以下.结论 该方法较国家标准方法操作简单,且灵敏度高,准确性、重现性好,适应于生活饮用水中痕量环氧氯丙烷的测定.
目的 建立同位素稀釋-氣相色譜質譜聯用方法測定生活飲用水中環氧氯丙烷.方法 在生活飲用水樣品中加入D5-環氧氯丙烷內標應用液,先用活性炭對環氧氯丙烷進行富集,活性炭經2739×g離心脫水10 min,最後加入1.0 ml丙酮浸泡1h併進行解吸,解吸液用氣相色譜-質譜法進行測定,同位素內標法定量,併對方法的檢測限精密度和準確度進行評價,用該方法對某市25批次飲用水中環氧氯丙烷進行測定.結果 採用該方法測定環氧氯丙烷,在0.0645～3.8700 μg/L範圍內線性良好,線性方程為Y=2.828X +4.91×10-2(r＞0.999),測定濃度為0.0806、0.3230、3.2300 μg/L時,環氧氯丙烷的RSD分彆為7.9％、4.7％、3.1％；加標平均迴收率在95.7％ ～98.7％之間,方法檢測限為0.015 μg/L,定量限為0.052 μg/L.檢測的25批飲用水中環氧氯丙烷含量均在檢測限以下.結論 該方法較國傢標準方法操作簡單,且靈敏度高,準確性、重現性好,適應于生活飲用水中痕量環氧氯丙烷的測定.
목적 건립동위소희석-기상색보질보련용방법측정생활음용수중배양록병완.방법 재생활음용수양품중가입D5-배양록병완내표응용액,선용활성탄대배양록병완진행부집,활성탄경2739×g리심탈수10 min,최후가입1.0 ml병동침포1h병진행해흡,해흡액용기상색보-질보법진행측정,동위소내표법정량,병대방법적검측한정밀도화준학도진행평개,용해방법대모시25비차음용수중배양록병완진행측정.결과 채용해방법측정배양록병완,재0.0645～3.8700 μg/L범위내선성량호,선성방정위Y=2.828X +4.91×10-2(r＞0.999),측정농도위0.0806、0.3230、3.2300 μg/L시,배양록병완적RSD분별위7.9％、4.7％、3.1％；가표평균회수솔재95.7％ ～98.7％지간,방법검측한위0.015 μg/L,정량한위0.052 μg/L.검측적25비음용수중배양록병완함량균재검측한이하.결론 해방법교국가표준방법조작간단,차령민도고,준학성、중현성호,괄응우생활음용수중흔량배양록병완적측정.
Objective To establish a method for determination of the epichlorohydrin in drinking water by isotope dilution gas chromatography-nass spectrometry(GC-MS).Methods The internal standard solution D5-epichlorohydrin was added in drinking water sample.The epichlorohydrin was firstly collected by active carbon,and the adsorbent was then centrifuged at 2739 × g for 10 min to remove water.Finally,the epichlorohydrin was desorbed by dipping the active carbon in 1.0 ml acetone for 1 h.The desorbed solution was tested by GC-MS and quantified with isotopic internal standards.The detection limit,precision and accuracy of the assay were evaluated.This method was adopted to detect the epichlorohydrin in drinking water for 25 batches in a city.Results The determination method of epichlorohydrin represented a good linear relationship in the range of 0.0645-3.8700 μg/L,the linear regression equation was Y =2.828X + 4.91 ×10-2 (r ＞ 0.999).When the epichlorohydrin concentration were 0.0806,0.3230 and 3.2300 μg/L,the relative standard deviations (RSD) were 7.9％,4.7％ and 3.1％,respectively.The average recoveries were from 95.7％ to 98.7％.The limit of detection (LOD) was 0.015 μg/L,limit of quantification (LOQ) was 0.052 μg/L.The content of epichlorohydrin in the 25 cases of drinking water was under the limit of detection.Conclusion The method is more simple than the national standard method,with high sensitivity,accuracy and good reproducibility,which is suitable for detection of the trace amounts of epichlorohydrin in drinking water.
