SN/T 4013-2013Determination of iprodione residues in foodstuffs for export - GC-MS method (English PDF)

Foreword

This standard was drafted in accordance with GB/T 1.1-2009 given rules.

This standard replaces SN 0708-1997 "cereals for export Iprodione Residue testing methods." this standard compared with SN 0708-1997, the main technical changes are as follows.

--- Scope increased rice, soybeans, pork, beef, chicken, milk, oranges, blueberries, spinach, onion, carrot, chestnut and tea Leaves, remove the brown rice;

--- Remove the sampling part of the contents;

--- Samples extracted from acetone, acetonitrile or modify acidic acetonitrile extract;

--- Sample purification by Florisil column is amended as N- secondary amine (PSA), octadecylsilane (ODS) and the GCB Dispersant;

--- Measurement method is modified by gas chromatography gas chromatography - mass spectrometry;

--- Lower limit of detection method consists of 0.05mg/kg revised to 0.01mg/kg.

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This standard is proposed and managed by the National Certification and Accreditation Administration Committee.

This standard was drafted. Heilongjiang People's Republic of China Exit Inspection and Quarantine.

1 Scope

This standard specifies the foods Iprodione Residue gas chromatography - mass spectrometry.

This standard applies to rice, soybeans, pork, beef, chicken, milk, oranges, blueberries, spinach, onion, carrot, chestnut and tea iso Iprodione residues detection and confirmation.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document.

Laboratory use specifications and test methods GB/T 6682 Analysis

3 Method summary

Sample remaining iprodione with an acidic acetonitrile or acetonitrile extract, the extract was N- secondary amine (PSA), octadecylsilane (ODS) of carbon black and graphite purification by gas chromatography - mass spectroscopy and confirmed, quantified external standard.

4 Reagents and materials

Unless otherwise specified, all reagents were of analytical grade water as a water GB/T 6682 regulations.

4.1 acetonitrile. chromatography.

4.2 acetic acid (99.5%).

4.3 acetone.

4.4 sodium acetate.

4.5 sodium chloride.

4.6 anhydrous magnesium. by burning 650 °C 4h, placed in the dryer set aside.

4.7 1% acetic acid in acetonitrile. Take 10mL acetic acid (4.2), was added 990mL of acetonitrile (4.1) and mix.

4.8 iprodione standards. Iprodione, CAS. 36734-19-7, purity of greater than or equal to 99%.

4.9 standard solution include.

a) Iprodione standard stock solution. accurately weighed amount of iprodione standards, dissolved in acetone (4.3) and dilute to 100mL brown Flask, a standard stock solution having a concentration of 100µg/mL, and this solution at -18 °C transferred to a storage reservoir bottle six Months.

b) an intermediate standard solution. Imbibe iprodione 12.5mL standard stock solution in 50mL brown volumetric flask, dilute with acetone Standard intermediate solution at a concentration of 25.0µg/mL, and this solution was transferred to the reservoir bottle storage for three months at -18 °C.

c) standard working solution. the preparation of an appropriate standard working solution with a blank sample matrix according to need before use.

4.10 GCB adsorbent. 120µm ~ 400µm.