翟有朋,顧云,張宗祥,楊文武,張永兵
(泰州市環境監測中心站,江蘇 泰州 225300)
·監測技術·
GC和HPLC測定水中苦味酸的比較
翟有朋,顧云,張宗祥,楊文武,張永兵
(泰州市環境監測中心站,江蘇 泰州 225300)
建立了氣相色譜法(GC)和高效液相色譜法(HPLC)測定水中苦味酸的分析方法,并對2 種方法進行比較。GC法檢出限為0.000 4 mg/L,線性范圍為0.0~0.050 mg/L,加標回收率為92.3%~94.1%,相對標準偏差為4.6%~8.9%。HPLC法檢出限為0.02 mg/L,線性范圍為0.10~5.00 mg/L,加標回收率為93.7%~96.5%,相對標準偏差為1.3%~2.0%。2種方法相比,GC法靈敏度較高,可用于痕量分析,但操作煩瑣,不能有效地將苦味酸與硝基酚類干擾物分離;而HPLC法雖然靈敏度較差些,但簡單、快速、穩定性好、準確度高,可有效地將苦味酸與硝基酚類干擾物分離。
苦味酸;氣相色譜法;高效液相色譜法;水;比較
Abstract: Two analysis methods of picric acid in water were established by gas chromatography and high performance liquid chromatography, and the advantages and disadvantages of two methods were compared.The method detection limit of GC was 0.000 4 mg/L, the linear range was 0.0~0.050 mg/L, the recovery of standard addition was 92.3% to 94.1%, the relative standard deviation was 4.6% to 8.9%. The method detection limit of HPLC was 0.02 mg/L, the linear range was 0.10~5.00 mg/L, the recovery of standard addition was 93.7% to 96.5%, the relative standard deviation was 1.3% to 2.0%. GC had higher sensitivity and was suitable for trace analysis, but its operation was complex, and it couldn't separate picric acid and other nitrophenolic distractors effectively. HPLC was simple and rapid,it had good stability and high accuracy, picric acid and other nitrophenolic distractors could be separated effectively by this method.
Keywords: Picric acid; Gas chromatography; High performance liquid chromatography; Water;Comparison
苦味酸(Picric acid)又稱2,4,6- 三硝基苯酚,俗稱黃色炸藥,是軍事上最早使用的一種烈性炸藥[1]??辔端釓V泛應用于工農業生產中,在醫藥上用作消毒劑,在農業上用作殺菌劑[2],在環保上用作溶解白色垃圾的良好溶劑。苦味酸會對人的眼睛、皮膚、呼吸道和消化道產生危害,長期接觸會引起頭暈、頭痛、記憶力下降等癥狀。
苦味酸作為《地表水環境質量標準》(GB 3838—2002)中規定的集中式生活飲用地表水源地80個特定項目之一,其標準限值為0.5 mg/L[3]。目前測定水中苦味酸常見的方法有氣相色譜法[4]、高效液相色譜法[5-6]、氣相色譜-質譜聯用法[7]和液相色譜-質譜聯用法[8-9]等。我國推薦的方法為《生活飲用水標準檢驗方法》(GB/T 5750.8—2006)[10]中規定的氣相色譜法,檢出限為1 μg/L,暫時還沒有標準推薦的高效液相色譜法?!?br>