DOI /j.issn Food Research And Development UPLC-MS/MS 5 0.

Size: px

Start display at page:

Download "DOI /j.issn Food Research And Development UPLC-MS/MS 5 0."

矶杨蒿
4 years ago
Views:

1 DOI /j.issn Food Research And Development UPLC-MS/MS 5. 1 mol/l ProElut PXC 5 % - Thermo Hypersil Gold mm 2.1 mm 1.9 μm ESI %~112.5 % RSD 4.1 %~11. % n= μg/kg 5 - Determination of 5 Opium Poppy Husk Alkaloids in Broth by Liquid Chromatography-Electrospray Tandem Mass Spectrometry GAO Zhi-ying 1 2 HONG Xia 1 2 LIU Qi 1 2 QIAN Ying-wen 1 2 ZHOU Xin-kui 1 2 HE Hai-ning Gansu Business Technology Institute Lanzhou 731 Gansu China 2. Gansu Zhongshang Food Quality Test and Detection Co. Ltd. Lanzhou 731 Gansu China Abstract A method for simultaneous determination of 5 opium poppy husk alkaloids in broth sample was developed by ultra performance liquid chromatography -electrospray tandem mass spectrometry. Broth samples were extracted by.1 mol/l hydrochloric acid then concentrated and purified by ProElut PXC solid-phase extraction column after that were eluted by 5 % ammonia-methanol.the separation was performed on a Thermo Hypersil Gold mm 2.1 mm 1.9 μm column and detected by mass spectrometry using electrospray ionization ESI in positive mode under multiple reaction monitoring mode.the recovery rates of the spiked sample was in the range of 71.8 % % and the relative standard deviation RSD was between 4.1 % to 11. % n =6. The detection limits for morphine codeine thebaine papaverine and narcotine were μg/kg and.4 μg/kg.this method can be successfully applied to the simultaneous detection for 5 opium poppy husk alkaloids in broth. Key words high performance liquid chromatography-tandem mass spectrometry broth solid-phase extraction alkaloid in opium poppy husk Morphine Codeine [1] Thebaine Papaverine Noscapine 2 139RTSA25 9FTGA18-15JTCA [2] 25

2 1.2.2 [3] 5 ml 5 ml 5 2 / ~3 / 5 ml 5 ml 65 kpa 5 min [4] 1 6 ml - 5 % [5-6] [7-8] [9-1] 15 ml [11] [12-13] [14-16] - [17-21] [22-3] [31] - 1 ml.22 μm Thermo Hypersil Gold mm 2.1 mm 1.9 μm.25 ml/min 2 μl 4 A.1 % B 1 1 ESI Table 1 Gradient elution table UltiMate 3/TSQ Quantum Access MAX Hypersil Gold mm 2.1 mm 1.9 μm Thermo CF16RX Hitachi VOR- TEX 3 IKA mivac GeneVac SB-52DTN ESI JJ MRM 3.5 kv ProElut PXC 2 mg 6 ml L/min 2 o2si Table 2-18 Fisher g.1 g ml 15 ml. 1 mol/l 1 min 4 8 r/min 5 min ml 1 ml 1 s UPLC-MS/MS 5 /min / ml/min A.1 % /% B /% L/min /153.1* 286.4/ /166.1* 3.6/ /59.8* 312.6/ /23.* 34.5/ /22.9* 414.3/25.9 * ESI-MS/MS analysis parameters 119 /min /V

3 PWC PLS PXC 71.8 %~112.5 % PWC 45.3 %~72.5 % PLS 33.4 %~68.2 % PXC SPE. 1 mol/l Thermo Hypersil Gold mm 2.1 mm 1.9 μm UPLC-MS/MS 5 5 PXC.1 % min QuEChERS QuEChERS 5 ESI PSA -N- 5 C % 3 /% /min A.

4 UPLC-MS/MS /% /min B. /% /min C. Fig.1 1 Total ion chromatograms of standard solution and sample

5 122 UPLC-MS/MS μg/l μg/l RSN % 63. % 77.3 % 62.2 % 68.3 % RSN Table Linear analysis detection limits and of five compounds / μg/kg / μg/kg / μg/kg y= x r= ~ y= x r= ~ y=23 943x r= ~ y= x r= ~..5.2 y= 647x r= ~ %~112.5 % 1 g RSD 4.1 %~11. % μg/kg μg/kg 6 4 ProElut PXC 4 5 n=6 Table 4 Recovery rates and precision of five compounds ESI / μg/kg /% RSD/% min %~112.5 % RSD 4.1 %~11. % n= μg/kg [1]. 215( )[M]. :,215:584 [2],,. 3 5 [J].,211,3(12): [3],,.

[J].,215,21(3):8-1 [19],,,. - [4].DB 31/21-212 [J].,212(4):2-252 - [2],,. - [S]. :,212 [J].,25,23(6):639-641 [5],,.ELISA [J]. [21],,. -,23,13(5):575-577 [6],, [J].,24,14(2):28-29 [7],,,. [J].,23,38(8):619-62 [8],,,1992,2(6):375 [9],, [J].

6 [J].,215,21(3):8-1 [19],,,. - [4].DB 31/ [J].,212(4): [2],,. - [S]. :,212 [J].,25,23(6): [5],,.ELISA [J]. [21],,. -,23,13(5): [6],, [J].,24,14(2):28-29 [7],,,. [J].,23,38(8): [8],,,1992,2(6):375 [9],, [J].,211,32(6): [1],,,.ELISA 1413 [22],,,. - 6 [J].,212,38 (8): [J]. [23],,,. /HPLC-MS/MS. PCR 725,. PCR 5 [J].,214, [J].,211,36(7):93-96,12 24(17): [11],,. [J]. [25],,,.QuEChERS/UPLC-MS,1994,4(3): [12],, [J].,2,1(1):38-4 [13],,,. [J].,215,25(14): ,231 [14],. [26],,. - - [27],,,. 5 -,.GC/MS [28],,,. - [J].,211,4(4): [15],, [J].,21,2(11): ,2788 [16],, [J].,215,25(2): [17]. UPLC-MS/MS 5 [J]. -,211,47(12):1411- [J].,214,33(6):722- [24],,,. - ( ) [J].,214,16(4): [J].,212,29(1):88 [J].,211,21(2): [J].,212,33(12):91-94.GC/MS [29],,,. - [J].,214,35(22): ,.GC/MS [3],,,. - [J].,21,31(7): [31],,,. - - [J].,27,17(1):72-73 [18],,,. - -HPLC [J]. ( ),29,29(3): [J].,214, 24(16): , !!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!

材料与方法仪器 ACQUITY UPLC Xevo TQ-S 三重四级杆液质联用仪 ( 美国 Waters 公司 ); 电喷雾离子源 (ESI), Masslynx 4.1 数据处理系统 (Waters);Thermo 低温离心机 ;KQ

材料与方法仪器 ACQUITY UPLC Xevo TQ-S 三重四级杆液质联用仪 ( 美国 Waters 公司 ); 电喷雾离子源 (ESI), Masslynx 4.1 数据处理系统 (Waters);Thermo 低温离心机 ;KQ [ 应用纪要 ] Rapid identification of 5 illegal additives in slimming health food by Xevo TQ-S 郝刚苏州市食品药品检验所, 苏州 15104 关键词超高效液相色谱 - 质谱, 多反应监测, 减肥类保健食品非法添加, 快速定性定量