| Objective: The lacidophilins preparations will be performed to obtain the current standard data for safety indicators such as chloramphenicol, melamine and addiction of lactobacillus fermentation metabolites. Detection method is established for the statistical analysis of lacidophilin preparations quality status. Analysis preparations which from the manufacturers of quality is to provide technical support for improving the quality of the supervision, inspection and the manufacturer.Methods: The first chapter according to the current standard test is access to a amount of data,and to obtain a sample of comprehensive quality analysis. The second chapter in national standard is after the improvement of the established lacidophilin preparations of chloramphenicol residue UPLC- MS/ MS detection method. Using the ACQUITY UPLC BEH HILIC C18 column, acetonitrile:water( 30: 70) as mobile phase, determination of lacidophilin preparations of chloramphenicol residue. The combination between the high performance liquid chromatography with higher speed and resolution and the triple quadrupoe LC- MS/ MS with higher selectivity and sensitivity will provide a powerful safe guard for the qualitative and quantitative analysis of the target compounds. The third chapter currently existing national standards GB/ T 22388- 2008 raw milk and dairy products of melamine determination method( the first method of high performance liquid chromatography), using high-performance liquid phase chromatography with ultraviolet detector, using a symmetry C18( 4.6 mm× 150 mm, 5 μm) column, from the buffer a phase( citric acid 2.132 g and octane sulfonic acid sodium 2.156 g, add about 980 m L dissolved in water, adjusted to p H 3.0, fixed volume to 1000 m L) : B phase acetonitrile( A: B=90:10) as mobile phase. In the fourth chapter, the high performance liquid chromatography, chirex 3126( D- penicillamine)- Phenomenex( 250 mm× 4.6 mm)column with 2 m M Cu SO4 solution- isopropanol( 95: 5) as mobile phase at the detection wavelength of 254 nm. Determination lacidophilin preparations of L- and Dlactate content and their ratio. In the fifth chapter using the rapid esterification method, after trifluoride boron- methanol methyl esterification by flame ionization detector( FID)- detector using HP- innowax( average molecular weight of polyethylene glycol PEG 15000)( 30 mm× 0.32 mm, 0.5 mm) column, the simultaneous determination of lacidophilin preparations of acetic acid,lactic acid and succinic acid. Results: The evaluation of the 237 batch of lacidophilin preparations,data statistical analysis showed that poor process stability individual manufacturers.Choosing twenty- one manufacturers of the 59 batch of lacidophilin preparations HPLC- MS was established for determination of chloramphenicol, and has a good linear relationship( r= 0.9994). The recovery rate is 102.84% ~ 117.71%, the relative standard deviation( RSD) ranges from 0.46% to 0.69%. The content of the national standard for determination of twenty- one kinds of 59 batches is lacidophilin preparations of melamine. The linear is( r= 1.0000), and the recovery rate is 99.16%~ 107.26%. Meanwhile the relative standard deviation( RSD) ranges from 0.94% to2.20%. The calibration curves of L- and R- lactic acid were linear with regressions being of 1.000 in the concentration range of 0.10~ 1.040 mg/ m L.The recovery of D-lactic acid and L-lactic acid was 96.13% ~ 97.75% and 95.07% ~ 100.00%. In addition, the RSD were 1.12% ~ 2.44% and 0.14% ~ 1.34%, respectively. The fifth chapter, using gas phase chromatography determination of 56 batches was lacidophilin preparations in acetic acid,lactic acid,and succinic acid content. The recovery rates were 115.01% ~ 112.95% and 87.84% ~ 91.68%, 86.29% ~ 93.04%.Conclusion: Routine inspection data analysis that process stability of G products was better meanwhile other manufacturers from poor stability analysis process of total acid and protein were indicators. The determination of lactic acid in the preparation of chloramphenicol linear good liquid chromatography mass spectrometry can be used for the determination of chloramphenicol in preparation of lacidophilin preparations in qualitative and quantitative. Application of HPLC method for the determination of melamine in lactobacillus preparation methodology experiment proved that a goodlinear range and high recovery, quantitative and qualitative analysis of melamine content is in lactobacillus preparation. Using high performance liquid chromatography, chiral separation of lactic acid, determination of content and the ratio of lacidophilin preparations were L- lactic acid and D- lactic acid. The method had a good linear range and recovery. The content of acetic acid, lactic acid and lactic acid in lacidophilin preparations were determined, which can be used for the quality evaluation of lacidophilin preparations by gas chromatography. |
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