SN 0645-1997Determination of diuron residues in meat and meat products for export. Liquid chromatography method (English PDF)

Foreword

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

This standard replaces SN 0645-1997 "export of meat and meat products diuron residues in." Compared with SN 0645-1997, the main technical changes are as follows.

--- The original standard name "export meat and meat products diuron residues in" to "export meat and meat products diuron Determination of the residual liquid chromatography ";

--- Cancel the original standard sampling and sample preparation section;

--- The original scope of application of the revised standard is. beef, canned luncheon meat, chicken meatballs, lamb, donkey;

--- Sample pretreatment conditions were revised;

--- Of liquid chromatography conditions were revised.

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

This standard was drafted. People's Republic of China Shandong CIQ.

1 Scope

This standard specifies the method for liquid chromatography export meat and meat products diuron residues.

This standard applies to beef, canned luncheon meat, chicken meatballs, lamb, donkey in the determination of diuron Long residues.

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 diuron methanol - acetonitrile (11, volume ratio) extraction by liquid-liquid partition and neutral alumina column purified, Determined by high performance liquid chromatography with UV detection, external standard.

4 Reagents and materials

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

4.1 Methanol. HPLC grade.

4.2 acetonitrile. HPLC grade.

4.3 chloroform. The all-glass apparatus redistilled.

4.4 petroleum ether. boiling range 60 °C ~ 90 °C, after all-glass apparatus redistilled.

4.5 anhydrous sodium sulfate. After burning 650 °C 4h, storage desiccator.

4.6 sodium chloride.

4.7 methanol - acetonitrile (11 volume). amount of an equal volume of methanol and acetonitrile, mixed well and reserve.

4.8 methanol - acetonitrile - water (70525, volume ratio). by volume of methanol, acetonitrile and water, mixed thoroughly take 70.5.25 volume ratio, and Degassed, filtered and set aside.

4.9 with saturated sodium chloride solution. adding an excess of sodium chloride in water, heated and boiled for 10min, until no more sodium chloride dissolved, cooled to room temperature. The cooled solution was filtered with filter paper, that is, saturated sodium chloride solution.

4.10 diuron (diuron) standard purity greater than or equal to 98.0%.

4.11 Standard stock solution (100mg/L). Weigh 10.0mg diuron standards, was dissolved in methanol - acetonitrile (4.7), and transferred 100mL flask with methanol - acetonitrile (4.7) to volume, mix, 0 °C ~ 4 °C preservation.

4.12 standard working solution. If necessary, draw a certain amount of standard stock solution (4.11), with methanol - into a series of diluted aqueous solution (4.8) - acetonitrile Standard working solution.

4.13 neutral alumina column. 6mL, 1000mg, or equivalent person. Before use 5mL methanol - acetonitrile - water (4.8) Pre-rinse.

4.14 over anhydrous sodium Column. 3g over anhydrous sodium sulfate and placed in a glass column tube.