SN/T 5324.2-2020 PDF English
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Determination of imipramine, carbamazepine, fluoxetine, flunixin and clomipramine in exported packaged drinking water and drinking natural mineral water - LC- MS/MS method
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SN/T 5324.2-2020: Determination of imipramine, carbamazepine, fluoxetine, flunixin and clomipramine in exported packaged drinking water and drinking natural mineral water - LC- MS/MS method
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/SNT5324.2-2020
Determination of imipramine, carbamazepine, fluoxetine, flunixin and
clomipramine in exported packaged drinking water and drinking
natural mineral water - LC- MS/MS method
Foreword
This standard is drafted according to GB/T 1.1—2009, GB/T 20001.4—2015 and SN/T 0001—2016.
Please note that some of the contents of this document may involve patents. The issuing body of this
document does not undertake the responsibility of identifying these patents.
This standard is proposed by and is under the jurisdiction of General Administration of Customs, P. R.
China.
The standard is drafted by Beijing Customs District P.R.China, Beijing Academy of Food Science,
Academy of Military Medical Sciences.
The main drafters of this standard are Wang Peiyue, Rao Hong, Feng Xin, Han Shen, Cui Fengyun, Liang
Nana, Qi Heming, Gu Jin, Liu Ying, Zhang Can.
Determination of imipramine, carbamazepine, fluoxetine, flunixin and
clomipramine in exported packaged drinking water and drinking
natural mineral water-LC-MS/MS method
1 Scope
This standard specifies the determination of imipramine, carbamazepine, fluoxetine, flunixin and clomipramine
in purified drinking water, natural drinking mineral water and other drinking water.
This standard is applicable to the determination of imipramine, carbamazepine, fluoxetine, flunixin and
clomipramine in purified drinking water, natural drinking mineral water and other drinking water.
2 Normative reference
The following document is necessary for this standard. For dated reference, only dated editions shall apply to this
standard. For undated references, the latest edition of the normative document referred to apply.
GB/T 33087 Ultra pure water for instrumental analysis specification and test methods
3 Terms and definitions
There is no term or definition to be defined in this document.
4 Principle
The samples are separated and determined by liquid chromatography-mass/mass spectrometry, and quantified by
external standard method.
5 Regents and materials
Unless otherwise specified, all the regents used should be chromatographic grade. “Water” is the ultra pure
water for instrument analysis prescribed by GB/T 33087.
5.1 Methanol.
5.2 Formic acid.
5.3 Acetonitrile.
5.4 Formic acid solution (0.1%): pipet 1 mL of formic acid, add water to 1 000 mL and mix well.
5.5 Imipraminestandard material:C19H24N2, CAS 50-49-7, purity ≥ 99%.
5.6 Carbamazepine standard material: C15H12N2O, CAS 298-46-4, purity ≥ 99%.
5.7 Fluoxetine standard material: C17H18F3NO, CAS 54910-89-3, purity ≥ 99%.
5.8 Flunixin standard material: C14H11F3N2O2, CAS 38677-85-9, purity ≥ 99%.
5.9 Clomipramine standard material: C19H23CIN2, CAS 303-49-1, purity ≥ 99%.
5.10 Standard stock solutions: separately weigh10 mg (accurate to 0.1 mg)imipramine (5.5), carbamazepine
9SN/T 5324.2—2020
(5.6), fluoxetine (5.7), fluonixin (5.8)and clomipramine (5.9), dissolve and fill to the volume of 10 mL
using methanol (5.1). The concentration of each standard in standard stock solution is 1000 mg/L. The standard
stock solutions storage at -18℃ .
5.11 Mixed standard intermediate solution: separately pipet 100 μL each standard stock solution (5.10)and
mix. Fill to the volume of 10 mL using methanol (5.1). The concentration of each standard is 10 mg/L. The
mixed standard intermediate solution storage at 4 ℃ .
5.12 Mixed standard working solution: take appropriate amount of mixed standard intermediate solution (5.11)
and dilute with water. The concentration of the standard series solution is 0.05 ng/mL, 0.1 ng/mL, 0.5 ng/mL,
2 ng/mL, 10 ng/mL and 20 ng/mL respectively. Prepare when it will be used.
6 Apparatus and equipment
6.1 UPLC-MS/MS: equipped with electric spray ion source (ESI).
6.2 Analytical balance: a sensitivity of 0.1 mg.
6.3 Centrifuge: rotational speed ≥ 10 000 r/min.
6.4 Plugged plastic centrifuge tube: 2 mL.
6.5 Nylonmillipore filter film: 0.22 μm.
7 Procedure
7.1 Sample preparation
The water samples are mixed and stand for about 10 min. Pipet a small amount of water into the 2 mL plugged
plastic centrifuge tube (5.4). After centrifugation (12 000 r/min, 5 min), filter the about 1 mL supernatant with
millipore filter film (5.5)for LC-MS/MS analysis.
7.2 Sample storage
The test samples should be stored at 4℃ .
7.3 Determination
7.3.1 UPLC operation conditions
UPLC operation conditions are as follows:
a) Mobilephase (A): Acetonitrile; mobilephase(B): 0.1% Formic acid water solution;
b) Chromatographic column: UPLC BEH C18, 100 mm×2.1 mm, 1.7 μm or equivalent;
c) Flow rate: 0.35 mL/min;
d) Injection volume: 10 μL;
e) Column temperature: 30 ℃ ;
f) Gradient elution: according to table 1.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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