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Determination of okadaic acid in shellfish meat for import and export. LC-MS/MS method
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SN/T 2269-2009
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Basic data | Standard ID | SN/T 2269-2009 (SN/T2269-2009) | | Description (Translated English) | Determination of okadaic acid in shellfish meat for import and export. LC-MS/MS method | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | X20 | | Classification of International Standard | 67.050 | | Word Count Estimation | 16,193 | | Date of Issue | 2009-02-20 | | Date of Implementation | 2009-09-01 | | Regulation (derived from) | National Quality Inspection [2009] No. 67 | | Issuing agency(ies) | General Administration of Customs | | Summary | This standard specifies the import and export of mussels and clams in okadaic acid sample preparation and liquid chromatography tandem mass spectrometry detection method. This standard applies to import mussels and clams in the detection of okadaic acid. | SN/T 2269-2009: Determination of okadaic acid in shellfish meat for import and export. LC-MS/MS method
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Determination of okadaic acid in shellfish meat for import and export.LC-MS/MS method
Exit inspection and quarantine industry standard book People's Republic of China
Detection and export shellfish meat okadaic acid
Liquid chromatography - tandem mass spectrometry
Posted 2009-02-20
2009-09-01 implementation
People's Republic of China
The State Administration of Quality Supervision, Inspection and Quarantine released
Foreword
The Standard Appendix A, Appendix B are informative appendices.
This standard is proposed and managed by the National Certification and Accreditation Administration Committee.
This standard was drafted. People's Republic of China Shanghai Entry-Exit Inspection and Quarantine Bureau.
The main drafters of this standard. Fang Xiaoming, Wang, Tang Yifeng, Wang Chuan now.
This standard is the first release of the entry-exit inspection and quarantine industry standards.
Detection and export shellfish meat okadaic acid
Liquid chromatography - tandem mass spectrometry
1 Scope
This standard specifies the import and export mussels and clams in okadaic acid sample preparation and liquid chromatography - tandem mass spectrometry.
This standard applies to detect and export mussels and clams in okadaic acid.
2 Determination
2.1 Method summary
Sample of okadaic acid with methanol/water extraction, chloroform extraction and then by Sep-paksilica solid-phase extraction (SPE),
By C18 column chromatography, choose positive electrospray ionization mass spectrometry mode, external standard.
2.2 Reagents and materials
Unless otherwise specified, the reagents were of analytical grade, double distilled water or deionized water to adapt.
2.2.1 acetonitrile. HPLC grade.
2.2.2 methanol.
2.2.3 formic acid.
2.2.4 n-hexane.
2.2.5 chloroform.
2.2.6 acetone.
2.2.7 Nitrogen. purity > 99.9%.
2.2.8 Methanol - water (80 + 20).
2.2.9 n-hexane - acetone - water (20 + 80 + 0.3).
2.2.10 methanol - acetone - water (3 + 97 + 0.3).
2.2.11 methanol - acetone - water (50 + 50 + 0.3).
2.2.12 0.1% aqueous formic acid solution (containing 2mmol/L ammonium acetate). 1L of water was added 0.156g 1.0mL of formic acid and ammonium acetate.
2.2.13 acetonitrile and 0.1% aqueous formic acid solution (containing 2mmol/L ammonium acetate) (30 + 70).
2.2.14 okadaic acid (Okadaicacid, C44H68O13, CAS number. 78111-17-8) standard substance. not less than 98.0% purity.
2.2.15 okadaic acid standard stock solution. accurately weighed amount of standard okadaic acid, methanol formulated as 10μg/mL of
Standard stock solution at -18 ℃ can be stored for six months. The stock solution can be diluted to a suitable concentration of an intermediate solution as needed.
2.2.16 okadaic acid matrix standard solution. draw the right amount of okadaic acid standard stock solution or intermediate solution needed
(2.2.15), with a blank sample extract was diluted into a matrix of standard working solution of appropriate concentration. Paul matrix standard working solution at -18 ℃
Deposit may be used for one week.
2.2.17 Sep-paksilica column. Before using a small column in advance with 10mL acetone (containing 0.3% water), 10mL of methanol (containing 0.3% water) and
10mL hexane - acetone - water (20 + 80 + 0.3) activated, a flow rate of 2mL/min.
2.3 instruments and equipment
2.3.1 Liquid chromatography - tandem mass spectrometry. equipped with electrospray ionization source.
2.3.2 Solid phase extraction device.
2.3.3 thermostat nitrogen blowing means.
2.3.4 homogenizer.
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