YC/T 405.5-2011 English PDF (YCT405.5-2011)

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YC/T 405.5-2011: Tobacco and tobacco products. Determination of multi-pesticide residues. Part 5: Determination of maleic hydrazide residue. High performance liquid chromatography method
YC/T 405.5-2011
YC
TOBACCO INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 65.160
X 87
Registration number. 33250-2011
Tobacco and tobacco products –
Determination of multi-pesticide residues –
Part 5. Determination of maleic hydrazide residue –
High performance liquid chromatography method
ISSUED ON. AUGUST 2, 2011
IMPLEMENTED ON. SEPTEMBER 1, 2011
Issued by. State Tobacco Monopoly Bureau
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle... 4 
4 Reagents and materials ... 4 
5 Instruments and apparatuses ... 5 
6 Sample preparation ... 6 
7 Operation steps ... 6 
8 Result expression ... 7 
9 Recovery ... 8 
10 Test report ... 8 
Appendix A (Informative) Chromatogram example ... 9 
Foreword
YC/T 405 “Tobacco and tobacco products – Determination of multi-pesticide
residues” is divided into five parts.
- Part 1. High performance liquid chromatography - tandem mass
spectrometry method;
- Part 2. Determination of organochlorine and pyrethroids pesticide – Gas
chromatographic method;
- Part 3. Gas chromatography - Mass spectrometry method and gas
chromatographic methods;
- Part 4. Determination of dithiocarbamate pesticide residues – Gas
chromatography-mass spectrometry method;
- Part 5. Determination of maleic hydrazide residue – High performance liquid
chromatography method.
This is Part 5 of YC/T 405.
This Part was drafted in accordance with the rules specified in GB/T 1.1-2009
AND GB/T 20001.4-2001.
Please note that some contents of this document may involve patents. The
issuing authority of this document does not undertake any responsibility of
identifying these patents.
This Part was proposed by the State Tobacco Monopoly Bureau.
This Part shall be under the jurisdiction of the National Tobacco Standardization
Technical Committee - Cigarette Institute Branch (SAC/TC 144/SC 1).
This drafting organizations of this Part. China National Tobacco Corporation -
Zhengzhou Tobacco Research Institute, National Tobacco Quality Supervision
and Inspection Center, China Tobacco Standardization Research Center,
Hongta Tobacco (Group) Co., Ltd., China Tobacco Hubei Industry Corporation.
The main drafters of this Part. Zhang Hongfei, Bian Zhaoyang, Hu Bin, Tang
Gangling, Liu Huimin, Wang Hongbo, Lu Sheming, Guo Junwei, Shen Jun.
Tobacco and tobacco products –
Determination of multi-pesticide residues –
Part 5. Determination of maleic hydrazide residue –
High performance liquid chromatography method
1 Scope
This Part of YC/T 405 specifies the high performance liquid chromatography
method for the determination of maleic hydrazide residue in tobacco and
tobacco products.
This Part applies to the determination of maleic hydrazide pesticide residues in
tobacco and tobacco products. As for this method, the detection limit is
0.66mg/kg AND the quantitative limit is 2.18mg/kg.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 6682 Water for analytical laboratory use – Specification and test
methods
YC/T 31 Tobacco and tobacco products – Preparation of test sample and
determination of water content – Oven method
3 Principle
The crushed sample in the hydrochloric acid solution is heated for reflux and
extraction, then the extract is purified in C18 SPE column AND eluted by sodium
hydroxide solution, AND the elution is detected by the liquid chromatographic
UV detector.
4 Reagents and materials
5.2 Electric heating mantle.
5.3 Precision pH meter.
5.4 Spherical condenser pipe.
5.5 Analytical balance, sensitivity is 0.0001g.
5.6 0.45μm aqueous filter membrane.
5.7 High performance liquid chromatography with UV detector.
6 Sample preparation
In accordance with YC/T 31, PREPARE sample and MEASURE the sample’s
moisture content.
7 Operation steps
7.1 Extraction
WEIGH about 5g of samples, accurate to 0.01g; PLACE it into a 250mL grinding
mouth round bottom flask; ADD 50mL of hydrochloric acid solution (4.5).
PLACE the round flask in an electric heating mantle (5.2); INSTALL a spherical
condenser pipe (5.4); HEAT it for reflux. CONTROL the reflux speed to make
the steam reach to the second ball of the condenser pipe; continuously HEAT
for reflux for 1h. After completion of reflux, LET it cool down to room temperature;
USE qualitative filter paper to filter sample; COLLECT the filtrate into a 100mL
volumetric flask; USE appropriate amount of hydrochloric acid solution (4.5) to
rinse the condenser pipe and the extracted sample; FITER the filtrate and
COMBINE it into this 100mL volumetric flask; USE hydrochloric acid solution
(4.5) to make the volume reach to the mark.
7.2 C18 column pretreatment
TAKE 2mL of methanol (4.4) and 2mL of 0.1mol/L sodium hydroxide solution
(4.6) to consecutively pre-rinse the C18 solid phase extraction column (5.1).
7.3 Purification
From the 100mL volumetric flask, accurately PIPETTE 2mL of extract (7.1) onto
the C18 solid phase extraction column (5.1); immediately COLLECT the effluent
component into a 5mL volumetric flask (4.6); USE 2mL of 0.1mol/L sodium
hydroxide solution to elute it; COMBINE the eluent into this 5mL volumetric flask;
USE sodium hydroxide solution (4.6) to make the volume reach to the mark;