Method for quickly identifying Daqu grades
A large-scale and graded technology, applied in character and pattern recognition, preparation of test samples, instruments, etc., can solve the problems of low detection sensitivity, poor repeatability, and low accuracy
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[0025] The preparation process of the Daqu sample is as follows: adding distilled water to the Daqu sample, grinding, centrifuging, taking the supernatant and adding it to the NMR tube, and then adding the heavy water containing 0.05% deuterated trimethylsilyl sodium propionate (TMSP) internal standard, Mix well, seal, refrigerate, to be tested, 1 The measurement conditions of H-NMR were as follows: the measurement frequency was 600.13 MHz, the temperature was 298 K, the scanning range was -5 to 15 ppm, the sampling point was 64 k, and the number of scanning was 64. The grinding process is as follows: grinding at 70 Hz for 300 s, with two cycles; the centrifugation process is: centrifugation at 10000 rpm for 10 min.
[0026] When using partial least squares discriminant analysis: use partial least squares discriminant analysis O2PLS-DA to analyze the data in the standard sample NMR integral database to establish a classification model; Unknown Daqu samples were identified.
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[0031] 1. Measure the sample to be tested
[0032] 1.1 Daqu Materials:
[0033] In this example, a total of 80 samples of Luzhou Huaiyu Koji Co., Ltd. were collected from Luzhou Huaiyu Koji Co., Ltd. with different storage periods. Among them, 65 samples were used as training sets and 15 samples were used as test sets. , esterification force, ammonia nitrogen, bulk density) were graded, and the details are shown in Table 1 below. The selected Daqu pieces were pulverized, passed through a 0.25mm aperture sieve, and stored in a -80°C cryogenic refrigerator for later use. Heavy water used in the test (D 2 O) and sodium deuterated trimethylsilyl propionate (TMSP-d4) were purchased from Cambridge Isotope Laboratory, and the NMR spectrum was measured by Bruker AVANCEIII 600MHz superconducting nuclear magnetic resonance spectrometer.
[0034] Table 1 Classification and statistics of Luxiang Daqu
[0035]
[0036] 1.2 Sample preparation:
[0037] The optimal method is confirme...
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