118 217 5 38 1 DOI 1.3969/j.issn.5-6521.217.1.28 Food Research And Development 1 2 1 2 1 2 1 2 1 2 1 2 1. 731 2. 731 - UPLC-MS/MS 5. 1 mol/l ProElut PXC 5 % - Thermo Hypersil Gold mm 2.1 mm 1.9 μm ESI 3 71.8 %~112.5 % RSD 4.1 %~11. % n=6 1.2.8.4.5.4 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 1 2 1. 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 %-112.5 % 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 1.2.8.4.5 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 9FTGA18-15JTCA17 1983 [2] 25
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 1.3-1.3.1 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 1 1.1 - UltiMate 3/TSQ Quantum Access MAX Hypersil Gold mm 2.1 mm 1.9 μm Thermo CF16RX Hitachi VOR- TEX 3 IKA mivac 1.3.2 GeneVac SB-52DTN ESI JJ MRM 3.5 kv ProElut PXC 2 mg 6 ml 2 32 12 L/min 2 o2si Table 2-18 Fisher 1.2 1.2.1 1 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 /%..25 9 1..25 9 1 4..25 1 9 5..25 1 9 5.1.25 9 1 6..25 9 1 1.5 L/min 5 2 1.83 286.4/153.1* 286.4/166.1 3.15 3.6/166.1* 3.6/215.9 3.89 312.6/59.8* 312.6/251.7 4.15 34.5/23.* 34.5/324.6 4.17 414.3/22.9* 414.3/25.9 * ESI-MS/MS analysis parameters 119 /min /V 57 4 43 23 15 24 26 29 22 38
12 2 2.1 2.1.1 PWC PLS PXC 71.8 %~112.5 % PWC 45.3 %~72.5 % PLS 33.4 %~68.2 % PXC SPE. 1 mol/l 2.2 2.2.1 5 5 Thermo Hypersil Gold mm 2.1 mm 1.9 μm UPLC-MS/MS 5 5 PXC.1 % - 2.1.2 5 5 min QuEChERS 2.2.2 QuEChERS 5 ESI PSA -N- 5 C18 1 5 % 3 /% 1 2 3 4 5 /min A.
UPLC-MS/MS 5 121 /% 1 2 3 4 5 /min B. /% 1 2 3 4 5 /min C. Fig.1 1 Total ion chromatograms of standard solution and sample
122 UPLC-MS/MS 5 2.3 2.4-2.4.1 5 25 2 μg/l 1 5 1 2 μg/l RSN 3 5 69.3 % 63. % 77.3 % 62.2 % 68.3 % RSN 1 5 3 Table 3 3 5 Linear analysis detection limits and of five compounds / μg/kg / μg/kg / μg/kg y=5 944.4x+13 27.7 r=.999 8 5.~. 1.2 4. y=8 727.4x+15 361 r=.999 2 5.~..8 2.7 y=23 943x+17 99.3 r=.999 5 1.~..4 1.4 y=96 14.5x+96 73 r=.999 7 1.~..5.2 y= 647x+19 89.2 r=.999 9 1.~..4.2 2.4.2 71.8 %~112.5 % 1 g RSD 4.1 %~11. % 3.5 2.5 1. μg/kg 3.1.5 2. μg/kg 6 4 ProElut PXC 4 5 n=6 Table 4 Recovery rates and precision of five compounds ESI.5 2.5 1.5 2.5 1.1.5 2..1.5 2..1.5 2. / μg/kg /% RSD/% 73.9 71.8 76.7 112.5 12.9 93.5 85.5 8.5 92.8 82.4 84.9 9.8 8.9 82.1 9.5 5.1 4.4 4.5 8.2 11. 4.6 7.7 9.1 4.1 5.6 8.7 6.8 7.8 1.3 5.6 5 min 5 3 71.8 %~112.5 % RSD 4.1 %~11. % n=6 1.2.8.4.5.4 μg/kg [1]. 215( )[M]. :,215:584 [2],,. 3 5 [J].,211,3(12): 1387-1391 [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].,211,32(6):47-413 [1],,,.ELISA 1413 [22],,,. - 6 [J].,212,38 (8):168-171. [J]. [23],,,. /HPLC-MS/MS. PCR 725,. PCR 5 [J].,214, [J].,211,36(7):93-96,12 24(17):2481-2484 [11],,. [J]. [25],,,.QuEChERS/UPLC-MS,1994,4(3):14-143 [12],, [J].,2,1(1):38-4 [13],,,. [J].,215,25(14):2296-2298,231 [14],. [26],,. - - [27],,,. 5 -,.GC/MS [28],,,. - [J].,211,4(4):512-513 [15],, [J].,21,2(11):2784-2785,2788 [16],, [J].,215,25(2):3466-3468 [17]. UPLC-MS/MS 5 [J]. -,211,47(12):1411- [J].,214,33(6):722- [24],,,. - ( ) [J].,214,16(4):284-287 [J].,212,29(1):88 [J].,211,21(2):363-365 [J].,212,33(12):91-94.GC/MS [29],,,. - [J].,214,35(22):2243-2246,.GC/MS [3],,,. - [J].,21,31(7):13-132 123 [31],,,. - - [J].,27,17(1):72-73 [18],,,. - -HPLC [J]. ( ),29,29(3): 291-294 5 [J].,214, 24(16):2337-234,2345 216-8-25!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!