雙固相萃取柱凈化-超快速液相色譜-串聯(lián)質(zhì)譜法同時測定貝類組織中全氟羧酸及其前體物質(zhì)
發(fā)布時間:2019-06-26 23:19
【摘要】:建立同時測定貝類中13種全氟羧酸類化合物、6種氟調(diào)聚飽和酸和3種氟調(diào)聚不飽和酸的超快速液相色譜-串聯(lián)質(zhì)譜分析方法。樣品經(jīng)90%乙腈溶液超聲提取,Oasis WAX和Envi-Carb雙固相萃取柱凈化,Kinetex XB-C_(18)色譜柱(2.1 mm×100 mm,2.6μm)分離,多反應(yīng)監(jiān)測負離子模式掃描,同位素內(nèi)標法定量。22種目標物在各自相應(yīng)質(zhì)量濃度范圍內(nèi)線性良好,相關(guān)系數(shù)不低于0.995,定量限為0.03~1.67 ng/g。基質(zhì)加標回收率在63.05%~127.18%之間,相對標準偏差為4.70%~17.1%。本方法實現(xiàn)了復(fù)雜貝類基質(zhì)(肌肉、肝臟、外套膜、鰓、性腺等)中PFCAs及其前體物質(zhì)的同時測定,采用雙柱凈化方式,大大降低了雜質(zhì)成分的干擾,部分化合物的靈敏度優(yōu)于現(xiàn)有方法,適用于貝類樣品中PFCAs及其前體物質(zhì)的監(jiān)控分析,為研究PFCAs前體物質(zhì)的生物轉(zhuǎn)化提供了新技術(shù)手段。
[Abstract]:A rapid liquid chromatography-tandem mass spectrometry (HPLC-MS) method for the simultaneous determination of 13 perfluorocarboxylic acids, 6 fluoropolymeric saturated acids and 3 fluoropolysaturated acids in shellfish was established. The samples were purified by ultrasonic extraction of, Oasis WAX and Envi-Carb with 90% acetonitrile solution, separated on Kinetex XB-C_ (18) column (2.1 mm 脳 100 mm, 2.6 渭 m), scanned by negative ion mode by multi-reaction monitoring, and quantified by isotope internal standard method. The 22 targets were linear in the corresponding mass concentration range, the correlation coefficient was not less than 0.99 5, and the quantitative limit was 0.03 鈮,
本文編號:2506588
[Abstract]:A rapid liquid chromatography-tandem mass spectrometry (HPLC-MS) method for the simultaneous determination of 13 perfluorocarboxylic acids, 6 fluoropolymeric saturated acids and 3 fluoropolysaturated acids in shellfish was established. The samples were purified by ultrasonic extraction of, Oasis WAX and Envi-Carb with 90% acetonitrile solution, separated on Kinetex XB-C_ (18) column (2.1 mm 脳 100 mm, 2.6 渭 m), scanned by negative ion mode by multi-reaction monitoring, and quantified by isotope internal standard method. The 22 targets were linear in the corresponding mass concentration range, the correlation coefficient was not less than 0.99 5, and the quantitative limit was 0.03 鈮,
本文編號:2506588
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