高效液相色譜-電噴霧串聯(lián)四級桿質(zhì)譜法檢測

1、 1094 分析化學(xué) 第 38 卷 11 YE X iao-Zhen( 葉小珍 , SHAO Jia -Q ing ( 邵加慶 , W ANG Jian( 王 堅 . Chinese General Practice ( 中 國全科 醫(yī)學(xué) , 2009, 12( 2: 160 162 12 N ithipatikom K, D icame lli R F, K ohler S, Gum ina R J, Fa lck J R , Ca m pbellW B, G ross G J. A nal . B iochem. , 2001, 292( 1: 115 124 13 T sikas D.

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4、A nal. B iochem. , 2007, 365( 1: 40 51 18 Y ang J , Schme lzer K, G eorg iK, H amm ock B D. A nal . Chem. , 2009, 81( 19: 8085 8093 19 R ogatsky E, Ste in D . R ap id Comm un M ass Spectrom. , 2005, 16( 11: 1757 1759 D eter m ination of A rachidonic A cid and Its Endogenous E icosanoid M etabolites

5、in M ice T issues U sing L iquid Chro m atography / E lectrospray Ionization Tandem M ass Spectrom etry * 1 GU Y an1, 2, SH I X ian -Zhe , Z HAO SuM in1, GU Qun1, LU X in1 , XU G uo W ang1 1 ( CAS K ey Laboratory of S eparation Science for A naly tical Chem istry, D alian Institu te of Che m ical Ph

6、y sics , Chinese A cademy of Sciences , D alian 116023 2 (D ep ar t m ent of Phar m aceuticalA naly sis, School of P har m acy, Shenyang Phar m aceutical U niver sity, Shenyang 110016 Abstract A reversed phase liqu id chrom atography / tandem m ass spectrom etry m ethod w as developed to si m ultane

7、ously ana lyze arach id onic ac id ( AA and its m etabo lites such as prostag land in s( PG s, th rom boxane ( TXB2 , epoxye icosatrieno ic acid s( EET s, d ihydroxyeicosatrieno ic acid s( DHET s and hydroxyeicosatetrae no ic ac id s( HETE s through the correspond ing cyc lo oxygenase , cy tochrom e

8、 P450, and lipoxygenase pathw ays in m ice t issues . E th y l acetate extract io n w as e m p lo yed for sa m ple preparation after sonicatio n in an ice bath , and th e organ ic phase w as dried under vacuum and d isso lved in m ethano l for the LCM S /M S ana ly sis . 22 standard compounds w ere

9、separated w ith in 50 m in usin g a grad ient elution of acetonitrile and w ater w ith 0 . 05 % form ic acid( V /V on a C18 co lum n ( 250 mm 4 . 6 mm, 5 m . PGB1 and deuter ium labeled 15-HETE-d8 and AA-d8 w ere used as interna l standards . M ass spectrom etric detection w as perfor m ed using neg

10、at iv e e lectrospray io nizat ion and mu lt ip le react io n m onitorin g . The m ethod w as validated and show n to be accurate( recovery va lu es 70 . 7 % - 123 . 0 % , prec ise ( RSD < 20 % and sensitiv e ( LOQ 3- 250 g /L . The m ethod w as applied to separate arachidon ic ac id ( AA and its

11、m etabo lites in lu ng , liv er and spleen t issues in m ice and quant ify e icosano id levels in lung t issue . T he results w ere 11 -HETE ( 58 . 3 11 . 6 ng / g , 15 HETE ( 52 . 6 15 . 5 ng / g , PGE2 ( 210 102 ng / g , PGD2 ( 20 . 3 13 . 9 ng / g , PG J2 ( 39 . 2 15. 9 ng / g , TXB 2 ( 58 . 3 28 . 4 ng / g , PGF2 ( 3 . 8 6 . 0 ng / g and AA ( 1980 5