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OBJECTIVE：To es tablish a method for the content determination of heavy metals [lead （Pb），cadmium（Cd）， copper （Cu）， mercury （Hg）] and harmful elements [arsenic （As）] in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules. METHODS ：The samples were conducted pretreatment by microwave digestion instrument and determined by inductively coupled plasma mass spectrometry （ICP-MS）using elements germanium ，indium，bismuth as internal standard. RESULTS ：The linear ranges of Pb ，As，Cu，Cd and Hg were 1-20，0.5-10，5-100，0.5-10 and 0.2-4 ng/mL， respectively （all r＞0.997）. The limits of detection （LODs） were 0.041 1，0.013 2，0.057 3，0.009 0，0.005 4 ng/mL， respectively. The limits of quantification （LOQs）were 0.137 0，0.044 0，0.191 0，0.030 0，0.018 0 ng/mL，respectively. RSDs of precision and repeatability tests were all less than 6％. RSDs of stability tests （28 h）of Pb ，As，Cu and Cd were all less than 5％， and that of stability test （28 h）of Hg was less than 7％. The average recoveries were 89.44％（RSD＝5.87％，n＝9），99.56％ （RSD＝5.46％ ，n＝9），96.12％（RSD＝4.62％ ，n＝9），105.82％（RSD＝2.80％ ，n＝9）and 90.23％（RSD＝3.59％ ，n＝9）， respectively. Five elements were all detected in 63 batches of samples ，and the contents of them were 0.191 0-1.527 6，0.002 5- 0.047 4，0.034 1-1.549 0，0.001 5-0.078 8 and 0.001 9-0.005 4 mg/kg，respectively. CONCLUSIONS ：The method is simple ， sensitive and accurate. It is suitable for simultaneous determination of 5 elements in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules.
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OBJECTIVE: To analyze and study the characteristic variables of wavelength in near-infrared spectroscopy of artificial cow-bezoar. METHODS: A method of near-infrared spectroscopy coupled with competitive adaptive reweighted sampling(CARS) was performed in characteristic variables of wavelength screening for the qualitative and quantitative researches, respectively. RESULTS: Some characteristic variables of wavelength, 0.48%-4.44% of all variables of wavelength, were screened out by CARS for different models. Not only the number of variables for building models decreased significantly, but also the index parameters for evaluating model became better. CONCLUSION: This method is suitable for quality evaluation and quality control for artificial cow-bezoar.
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A LC-MS method was established for study of characteristic ions in frequently-used traditional Chinese medicinal materials derived from animal bile. UPLC-Q-TOF was used in the data acquisition work, then, the software of MarkerLynxTM v.4.1 was performed in the chemometric analysis of data. Besides, selected ion chromatograms of these bile acid ions were comparative studied. Better results were gained in the specificity identification of pig bile, bear bile, cultivated cow-bezoar , artificial cow-bezoar and some compound preparations(Hugan tablet and Rengongniuhuang Jiaxiaozuo capsule) by this method. The method is suitable for the specificity identification of pig bile, bear bile, cultivated cow-bezoar , artificial cow-bezoar and compound preparations containing these medicinal materials.
Subject(s)
Animals , Cattle , Bezoars , Bile , Chemistry , Chromatography, High Pressure Liquid , Ions , Chemistry , Mass Spectrometry , Medicine, Chinese Traditional , Species Specificity , Swine , UrsidaeABSTRACT
An HPLC-ELSD method for quantitation of GCANa, CA, HDCA, CDCA and DCA in artificial cow-bezoar was developed in this study. The chromatographic separation was performed using a Wondasil CC₁₈(4.6 mmχ250 mm，5 μm) column at a column temperature of 25 °C and liquid flow-rate of 1.0 mL·min⁻¹. Acetonitrile and 0.2% formic acid solution were used as mobile phase with a linear gradient and injection volume was 10 μL. An ELSD was used with a nitrogen flow-rate of 2.3 L·h⁻¹at a drift tube temperature of 110 °C. Some chemometric methods were applied in data procession and analysis for exploration of the markers of quality difference. The accurate and simple method is suitable for the quality evaluation and the quality control of artificial cow-bezoar.
Subject(s)
Animals , Cattle , Bezoars , Chromatography, High Pressure Liquid , Medicine, Chinese Traditional , Quality ControlABSTRACT
A method of thin-layer fingerprinting chromatogram of artificial cow-bezoar was established with the developing solvent consisting of cyclohexane, ethyl acetate, acetic acid and methanol (2∶7∶1∶2), and 10% sulfuric acid ethanol solution sprayed as colour-developing agent. After heated at 105 ℃, TLC was recorded as an image in ultraviolet light at 366 nm which was converted into grayscale. By the gray value extracted from the grayscale, the multivariate data obtained from TLC of samples could be analyzed by chemometric method. The results indicated that samples from different manufacturers could be distinguished by this method and some specific bands were found out. All in one, this simple and practical method was suitable for the evaluation of quality difference.
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Objective:To establish an HPLC method for the determination of p-aminophenol in pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules. Methods: A CAPCELL PAK MGⅡC18 (150 mm × 4. 6 mm,5 μm) chromatographic column was used with 0. 05% ammonium acetate solution-methyl (85∶ 15) as the mobile phase at the flow rate of 1 ml·min-1 , the detection wavelength was 232nm,the injection volume was 10μl,and the column temperature was 30℃. Results:The linear range of p-aminophenol was 9. 878 4-197. 568 0 ng(r = 0. 999 1), the average recovery was 99. 8%(RSD = 0. 9%,n= 9), and detection limit was 2ng. Conclusion:The method is simple, specific and accurate, which can be used to determine the contents related substances in of pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules.