ABSTRACT
OBJECTIVE: To establish a method for the quality control of cattle bile powder based on cholic acid components, evaluate the quality of commercially sold cattle bile powder, and analyze the possible adulteration. METHODS: A method was established for simultaneous determination of cholic acid content in bile powder of cattle, sheep, pig, chicken, duck and other animals. Self-made samples and samples collected by enterprises were studied respectively. Based on self-made samples, the differences and content rules of bile powder of cattle, pig, sheep and other animals were investigated, and the quality and possible adulteration of samples collected by enterprises were evaluated. RESULTS: An HPLC-ELSD method was established for simultaneous determination of 12 cholic acids in bile powder of cattle, sheep, pigs, chickens and ducks. By analyzing the determination results of 23 batches of self-made animal bile powder, the contents of cholic acid in cattle bile powder and other animal bile powder were determined. By analyzing the determination results of cattle bile powder samples collected from 23 enterprises, it was found that there were mainly two kinds of adulteration of cattle bile powder likely: sheep bile powder and cholic acid waste. Only 8 of the 23 batches of samples collected by enterprises met the requirements, and the qualified rate was only 34.8%. The quality of varieties needs to be improved and supervised urgently. CONCLUSION: The method established in this study can effectively control the quality of cattle bile powder, identify possible adulteration of cattle bile powder, and provide reference and basis for improving the quality standard of cattle bile powder and strengthening market supervision.
ABSTRACT
An HPLC-ELSD method with good specificity and good accuracy was used for the studies of fingerprint and quantification of multi-components for cattle bile powder. The chromatographic analysis was carried out on a Phenomenex Gemini C18 column (4.6 mm×250 mm, 5 µm) with a column temperature of 40 â and a liquid flow-rate of 1.0 mLâ¢min⻹ using 10 mmol ammonium acetate solution and acetonitrile as the mobile phase with a linear gradient. An ELSD was used with a nitrogen flow-rate of 2.8 Lâ¢h⻹, at a drift tube temperature of 110 â. The average contents of glycocholic acid, glycodeoxycholic acid, taurocholic acid, taurodeoxycholic acid were (25.2±17.0)%, (4.1±3.4)%, (24.5±20.0)% and (5.2±3.8)% respectively, and the total content of the four bile acids was (59.0±26.0)%. Beyond that, the preprocessing and pattern recognition analysis of the chromatographic fingerprints of samples were applied with chemometric method. The results of this chemometric analysis indicated that the samples from market and self-made samples were different signally, and four regions were noteworthy due to their great impact with poor chromatographic signal. All in one, because this HPLC-ELSD method was simple and accurate, it was suitable for the quality assessment and quality control of cattle bile powder and could be the technological base for its standard perfection.
Subject(s)
Bile/chemistry , Chromatography, High Pressure Liquid , Animals , Cattle , Quality Control , Sensitivity and SpecificityABSTRACT
An HPLC-ELSD method with good specificity and good accuracy was used for the studies of fingerprint and quantification of multi-components for cattle bile powder. The chromatographic analysis was carried out on a Phenomenex Gemini C₁₈ column (4.6 mm×250 mm, 5 μm) with a column temperature of 40 ℃ and a liquid flow-rate of 1.0 mL•min⁻¹ using 10 mmol ammonium acetate solution and acetonitrile as the mobile phase with a linear gradient. An ELSD was used with a nitrogen flow-rate of 2.8 L•h⁻¹, at a drift tube temperature of 110 ℃. The average contents of glycocholic acid, glycodeoxycholic acid, taurocholic acid, taurodeoxycholic acid were (25.2±17.0)%, (4.1±3.4)%, (24.5±20.0)% and (5.2±3.8)% respectively, and the total content of the four bile acids was (59.0±26.0)%. Beyond that, the preprocessing and pattern recognition analysis of the chromatographic fingerprints of samples were applied with chemometric method. The results of this chemometric analysis indicated that the samples from market and self-made samples were different signally, and four regions were noteworthy due to their great impact with poor chromatographic signal. All in one, because this HPLC-ELSD method was simple and accurate, it was suitable for the quality assessment and quality control of cattle bile powder and could be the technological base for its standard perfection.
