Determination of chromium content in hollow capsules by graphite furnace atomic absorption spectrometry - Master's thesis - Dissertation

Determination of chromium in hollow capsules by graphite furnace atomic absorption spectrometry

Key words: atomic absorption spectrometer; chromium content of hollow capsule; ; AA1800H April 15, 2012, CCTV "Weekly Quality Report", the current program "The Secret in the Capsule", exposed some enterprises in Hebei The leather waste was treated with quicklime and made into industrial gelatin. It was sold to some enterprises in Shaoxing Xinchang to make medicinal capsules, and finally flowed into the pharmaceutical company and entered the patient's abdomen. Since the leather is used in industrial processing, it is necessary to use a chromium-containing bismuth preparation, so that the capsule thus produced tends to have a heavy metal chromium exceeding the standard. After testing, 13 batches of drugs in some pharmaceutical factories, the heavy metal chromium content of the capsules used exceeded the standard. Since the main raw material of industrial gelatin is leather products, tanning is the most critical process in tanning production, and the chrome tanning method (the main active ingredient is chromium oxide). , about 12%) since its inception, due to its superior tanning performance has always occupied the dominance of tincture. Therefore, it is currently believed that the excessive content of chromium (Cr) is the main difference between the identification of industrial gelatin and edible gelatin. China's 2010 edition of the pharmacopoeia for gelatin gel strength, pH, light transmittance, conductivity, sulfite, peroxide, loss on drying, ignition residue, chromium content, heavy metal content, arsenic salt, microbial limits and other indicators There are clear rules. At present, the state has exposed some companies to produce gelatin with blue suede for their own economic interests, regardless of the health and safety of the public. In order to pursue profits, some hollow capsule enterprises use inferior gelatin as raw materials to produce hollow capsules in extremely poor conditions. Blue mink contains a lot of chromium and cannot be removed. Chromium is highly toxic to the human body. Low concentrations of chromium in the environment can cause subacute chronic poisoning, and dust can cause diseases such as pneumonia, ulcers and lung cancer. The 2010 edition of the Pharmacopoeia clearly states that the chromium content of medicinal gelatin should not exceed 2 mg/Kg. The chrome content evaluation solution for medicinal hollow capsules is introduced with reference to the 2010 edition of the Chinese Pharmacopoeia for the detection of chromium poison capsules for reference by relevant industries. In addition, it also provides comprehensive support for users in the after-sales service and technical application of the instrument, and provides guarantee for faster and better analysis and testing. 1. Main equipment and consumables Atomic absorption spectrophotometer AA1800H US analysis (China) Co., Ltd. Nitrate excellent pure Chinese medicine reagent chromium standard substance 1000ppm Non-ferrous metal research institute ammonium dihydrogen phosphate excellent grade pure Chinese medicine reagent 2 Sample preparation: Reference 2010 The annual edition of the Chinese Pharmacopoeia stipulates methods: weigh about 0.5 g of hollow capsules, place them in a 100 ml PTFE digestion tank, add 5-10 mL of concentrated nitric acid, mix well, cover the inner lid, tighten the jacket, set In the electric oven, heat digestion is carried out, and the temperature is controlled at 120--140 °C. After the digestion is complete, the digestion tank is placed on a hot plate, heated slowly at 120 ° C until the reddish brown vapor is exhausted and dried, filtered, and then transferred to a 25 mL plastic volumetric flask with 1% nitric acid, and the volume is adjusted to the mark. Shake well and test. The blank was prepared by the same method. 3 Instrument analysis conditions: Instrument conditions: lamp current: 4mA graphite tube type: pyrolysis coating wavelength: 357.9nm injection volume: 20ul slit: 0.2nm matrix improver injection volume: 5ul lighting mode: BGC-D2 heating program : Graphite furnace temperature program (pyrolysis graphite tube) stage # Temperature (°C) Time (sec) Heating method Sensitivity Gas path type Gas path (L/min) 1 150 30 RAMP Low argon gas 0.32 250 15 RAMP Low argon gas 0.33 350 10 RAMP Low Argon 0.74 400 10 RAMP Low Argon 0.75 550 5 RAMP High Argon 0.06 2200 3 STEP High Argon 0.07 2300 2 STEP Low Argon 1.0 Note: For chromium detection of pharmaceutical capsules, see Food Testing Standard GB/ The method of T 5009.123-2003 is processed. The sample processing method is dry ashing method and high pressure digestion method. The above introduction method is high pressure digestion method, which has the advantages of fast sample digestion speed, no pollution and loss, convenient operation and accurate measurement. Key words: atomic absorption spectrometer; chromium content of hollow capsule; aesthetic analyzer ; AA1800H

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