Quality control methods for
Preparation of standard stain
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- Limit test for cadmium and lead
- Recommended procedure Apparatus
- Preparation of the sample
Preparation of standard stain
Add 10 ml of stannated hydrochloric acid (~250g/l) AsTS and 1 ml of dilute arsenic AsTS to 50 ml of water. The resulting solution, when treated as described in the general test, yields a stain on mercuric bromide paper AsR referred to as the standard stain (10 µg of As). Limit test for cadmium and lead The method of determination is left to the analyst. Nevertheless, the determination must be consistent and sensitive enough to allow comparison with a reference material. Quality control methods for medicinal plant materials Recommended procedure Apparatus The equipment consists of a digestion vessel, consisting of a vitreous silica crucible (DIN 12904), "tall form", height 62mm, diameter 50mm, capacity 75ml, with a vitreous silica cover. Materials used are: - digestion mixture: 2 parts by weight of nitric acid (~1000g/l) TS and 1 part by weight of perchloric acid (~1170g/l) TS. - reference materials: olive leaves (Olea europaea) 1 and hay powder 2 . Clean scrupulously with nitric acid (~1000g/l) TS the digestion vessel and all other equipment to be used for the determination, rinse thoroughly several times with water and dry at 120°C. Preparation of the sample For the wet digestion method in an open system, place 200-250mg of air-dried plant material, accurately weighed, finely cut and homogeneously mixed, into a cleaned silica crucible. Add 1.0ml of the digestion mixture, cover the crucible without exerting pressure and place it in an oven with a controlled temperature and time regulator (computer-controlled, if available). Heat slowly to 100°C and maintain at this temperature for up to 3 hours; then heat to 120°C and maintain at this temperature for 2 hours. Raise the temperature very slowly to 240°C, avoiding losses due to possible violent reactions especially in the temperature range of 160-200°C, and maintain at this temperature for 4 hours. Dissolve the remaining dry inorganic residue in 2.5 ml of nitric acid (~1000g/l) TS and use for the determination of heavy metals. Every sample should be tested in parallel with a blank. Method The contents of lead and cadmium may be determined by inverse voltametry or by atomic absorption spectrophotometry. The following maximum amounts in dried plant materials, which are based on the ADI values, are proposed: - lead, 10 mg/kg; - cadmium, 0.3 mg/kg. 1 BCR reference material CRM No. 62 Community Bureau of Reference, obtainable from BCR, Directorate-General X11, Commission of the European Communities, 200 rue de la Loi, B-1049 Brussels, Belgium. 2 Obtainable from IAEA/V-10, International Atomic Energy Agency, Analytical Quality Control Services, Laboratory Geibersdorf, P.O. Box 1'00, A-Vienna, Austria. |
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