Billig Ed Hardy Liquid chromatography - mass spect

Liquid chromatography - mass spectrometry determination of the race was set in traditional Chinese medicine, music general standing, promethazine, hydroxyzine


DTrapSLESIXDB-C150 × 2.1mm. Ultrasonic cleaning instrument SK250LH. 1.3 Methods 1.3.1 Preparation of standard solution Weigh accurately a certain amount of game was set, music general standing, promethazine, hydroxyzine standard, constant volume with methanol, the preparation of a concentration of 1000mg / L of standard stock solution, accurately Pipette 1ml stock solution to 100ml flask, paired with a constant volume of methanol concentration of about 1mg / L mixed standard solution. 1.3.2 Sample Preparation Weigh accurately 1, solid samples, 1.0g, add 10.0ml methanol ultrasonic extraction 15min, filtered and diluted for use. 2, the liquid sample: direct methanol diluted sample by adding filter back off before use 0.2um membrane. 1.3.3 Liquid chromatography-mass spectrometry mass spectrometry conditions: nitrogen pressure 0.7kpa, flow rate of 8m ~ min, helium pressure 0.6mpa; positive ion mode; hydrazine ion scanning range m/z50 ~ 600; collision voltage in order as; ESI electrospray ionization source. Stop Time: 42.00min; flow rate: 0.3m ~ min; injection volume: 3l; column temperature: 30 ℃. Qualitative samples using full-scan mode,Billig Ralph Lauren Polos, mass spectra and retention time using qualitative. Selected two samples of quantitative ion mode using single-point calibration quantitative. Characteristic ions were (m / z) match was set: 243,196; song general standing: 208,115; [Author] at Davidson (1964 A), male, master, deputy director of the technicians, principally engaged in the study of physical and chemical testing . LC conditions: promethazine: 194,223; hydroxyzine: 201,166 2 Results and discussion 2.1 race was set, music general standing, promethazine, hydroxyzine qualitative match was set for the Figure 1,Ralph Lauren Pullover, curve general standing,Ralph Lauren polos, promethazine, hydroxyzine full scan of the Lc-MS chromatogram, can be seen from the figure, race was set, music general standing, promethazine, hydroxyzine can be well separated, according to the single The retention time of standard sample can be determined, four peaks are the song & P standing, promethazine, race was set, hydroxyzine. 2 to 9 are the race was set, scores standing, promethazine, hydroxyzine primary, secondary mass spectrum. Therefore, the qualitative identification of retention time and mass must be used together to determine. Scores standing 29j36237.5106 race was set hydroxyzine promethazine Ik-~ L. . . . . . V time (min) Figure 1 race was set, music general standing, promethazine, hydroxyzine total ion current 1o0 2 race was set for a mass spectrum of Chinese Journal of Health Laboratory 2o05 October 15 No. 10 period ChineseJoumMofHeMthIJabnmt0ryTechnolo ~, Oct2o05; Vol15N0101223200400 3 race was set for two spectra 200400H Figure 4 general standing of a mass spectrum 100 200 300 400 Figure 5 general standing of the two spectra 1002003004O0 canthus of a mass promethazine Figure 6 Figure 7 isopropyl howl of MS2 Figure 8 hydroxyzine a mass spectrum 2o04006oo Figure 9 hydroxyzine MS2 Figure 2.2 Linear range and detection limit were taken 1mg / L of the race was set, Qu P standing, promethazine, hydroxyzine 1,3,5 mixed standard solution peak area of ​​standard linear regression, correlation coefficient> 0.999; instrument detection limits were 0.1ng, 2Pg, 0.1ng, 1.1Pg (ON = 3); method detection limit of 1,0. o2 ... 1001mg/kg (ON = 3). 2.3 The recovery order to verify the reliability of the method, this paper three different extracellular matrix (bone pills, Xiangshayangwei granules,Billig Ed Hardy, oral liquid) samples as a background, samples were added to the three levels of standard solution, measured six times each level, do standard addition recovery experiment, the experimental results shown in Table 1. The results show that this method is more fixed on the game, scores standing,Ed Hardy shirt Wangjiang city pollution of the env, promethazine, hydroxyzine in three different substrates with high recovery and precision. Table 1 The recovery 2.4 The application of the method the method we use to purchase this paper on the market l9 proprietary Chinese medicines were determined, there is not a detected event was set, music general standing, promethazine, OH hydrochloride. [
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