OBJECTIVETo understand the content status of ethyl carbamate (EC) in yellow rice wine and the changes in storage period and shelf life in Zhejiang province.

METHODSA total of 475 samples of yellow rice wine purchased randomly from supermarkets and food stores in Zhejiang province during 2008-2012, and 49 samples collected from manufacturers were measured for EC content. The sample collected from manufacturers by filter sterilization was placed at 4 °C, room temperature and 37 °C for 400 d, respectively;a bottled wine and a wine in bag were bought from market were placed for 400 d in room temperature to conduct shelf life storage test, and measure the content in every point in 2011. The EC of the samples was determinated by gas chromatography-mass spectrometry after the samples were diluted with D5-EC isotope dilution technique, and purified by alkaline diatomite solid phase extraction column.

RESULTSThe overall detection rate of EC was 99% (472/475) in yellow rice wine of Zhejiang province in 2008-2012, the median value was 70-112 µg/kg, the 90th percentile was 190-333 µg/kg, the 95th percentile was 214-393 µg/kg, and the maximum value was 430-515 µg/kg. The content of EC was increased gradually along with the increasing of storage age in commercially yellow rice wine, and the average content of EC were positively correlated with storage age(r = 0.988). The contents of EC in yellow rice wine after sterilization increased from 74 µg/kg to 86 µg/kg, 127 µg/kg and 509 µg/kg at 4 °C, room temperature and 37°C, respectively for 400 d storage, the differences had statistical significance (F = 14.73, P < 0.01). The content of EC in yellow rice wines in shelf life, which stored in room temperature with bottle and bag package, was decreased slightly with increasing storage time in the beginning, from 215 to 184 µg/kg and 196 to 158 µg/kg, respectively, and increased again with increasing storage time after 250 d, with 252 µg/kg and 210 µg/kg in bottle and bag package after 400 d, respectively, the differences had statistical significance (Z = 2.37, P < 0.05).

CONCLUSIONEC is widespread in rice wine, the content of EC was correlated with storage time and temperature.

China ; Oryza ; Urethane ; analysis ; Wine ; analysis

OBJECTIVETo establish the method of simultaneous determination of methylcarbamate (MC) and ethylcarbamate (EC) in yellow rice wine by gas chromatography-mass spectrometry (GC/MS).

METHODSMC and EC in yellow rice wine were derived by 9-xanthydrol, and then the derivants were detected by GC/MS; and quantitatively analyzed by D5-EC isotope internal standard method.

RESULTSThe linearity of MC and EC ranged from 2.0 µg/L to 400.0 µg/L, with correlation coefficients at 0.998 and 0.999, respectively. The limits of quantitation (LOQ) and detection (LOD) were 0.67 and 2.0 µg/kg. When MC and EC were added in yellow rice wine at the range of 2.0-300.0 µg/kg, the intraday average recovery rate was 78.8%-102.3%, relative standard deviation was 3.2%-11.6%; interday average recovery rate was 75.4%-101.3%, relative standard deviation was 3.8%-13.4%. 20 samples of yellow rice wine from supermarket were detected using this method, the contents of MC were in the range of ND (no detected) to 1.2 µg/kg, the detection rate was 6% (3/20), the contents of EC in the range of 18.6 µg/kg to 432.3 µg/kg, with the average level at 135.2 µg/kg.

CONCLUSIONThe method is simple, rapid and useful for simultaneous determination of MC and EC in yellow rice wine.

Carbamates ; analysis ; Food Contamination ; analysis ; Gas Chromatography-Mass Spectrometry ; methods ; Oryza ; Urethane ; analysis ; Wine ; analysis

Ethyl carbamate (EC) as a potential carcinogen commonly exists in traditional fermented foods. It is important eliminate urea that is the precursors of EC in many fermented foods, including Chinese Rice wine. On the basis of achieving high-level overexpression of food-grade ethanol-resistant acid urease, we studied the hydrolysis of urea and EC with the recombinant acid urease. Recombinant acid urease showed degraded urea in both the simulated system with ethanol and Chinese Rice wine (60 mg/L of urea was completely degraded within 25 h), indicating that the recombinant enzyme is suitable for the elimination of urea in Chinese Rice wine. Although recombinant acid urease also has degradation catalytic activity on EC, no obvious degradation of EC was observed. Further investigation results showed that the Km value for urea and EC of the recombinant acid urease was 0.7147 mmol/L and 41.32 mmol/L, respectively. The results provided theoretical foundation for realizing simultaneous degradation of urea and EC.
Oryza ; Recombinant Proteins ; metabolism ; Urea ; chemistry ; Urease ; metabolism ; Urethane ; chemistry ; Wine ; analysis

Scutellariae Radix(Huangqin) is a well-known traditional Chinese medicine(TCM) used for the treatment of clearing heat in clinical application. It is bitter-cold by using directly, but the bitter-cold property can be relieved after wine-frying. The study of taste changes before and after wine-frying of Scutellariae Radix is of great significance in identifying Scutellariae Radix and wine-processed Scutellariae Radix and clarifying the traditional theory of wine-processing. In this experiment, 10 batches of Scutellariae Radix and wine-processed Scutellariae Radix were prepared. The contents of 5 flavonoids were determined by high performance liquid chromatography(HPLC), and principal component analysis(PCA) was performed with 5 flavonoids as variables. As a result, the contents were different in different batches of Scutellariae Radix, but Scutellariae Radix and wine-processed Scutellariae Radix could not be distinguished. Five sensory attributes(sour, salty, fresh, sweet, and bitter) were evaluated by artificial tasting, and the response values of 7 sensors(AHS, AHS, PKS, CTS, NMS, CPS, ANS, SCS) representing the taste of pieces were detected by electronic tongue. The correlation between sensory evaluation and response values of the electronic tongue were analyzed, and the results showed that the sensory evaluation of sour, salty, fresh, sweet, bitter and AHS, CTS, NMS, ANS, SCS sensors had different degrees of correlation, indicating that the electronic tongue technology can be used as an alternative to artificial taste and can serve as a means for quantifying the taste, and it can be used to evaluate the taste of TCM pieces. The taste method was used to analyze the response values of the electronic tongue, and the results showed that the bitterness of wine-processed Scutellariae Radix decreased and the salty taste increased. PCA was used to analyze taste changes before and after wine-processed Scutellariae Radix, and the results showed that taste differences between 2 pieces were divided into 2 categories. PCA loading scattering plots showed that response of saltiness and bitterness were the major factors to affect overall taste in Scutellariae Radix and wine-processed Scutellariae Radix. Based on electronic tongue response values, the Fisher discriminant model for Scutellariae Radix and wine-processed Scutellariae Radix was established, which showed that it could effectively discriminate them with a recognition rate of 100%. The experimental results showed that the electronic tongue combined with multivariate statistical analysis can be used to evaluate taste of TCM, at the same time, it could provide a fast and simple method for identifying different processed products.
Chromatography, High Pressure Liquid ; Medicine, Chinese Traditional ; Scutellaria baicalensis ; Taste ; Wine ; analysis

To determine the content of extracts in different processed products of Chuanxiong Rhizoma and the content of chlorogenic acid, ferulic acid, senkyunolide Ⅰ, coniferyl ferulate, senkyunolide A and ligustilide, in order to study the effect of different proces-sing methods on the alcohol-soluble extract and the content of six ingredients of Chuanxiong Rhizoma. The extract was determined according to the alcohol-soluble extract determination method set forth in item 2201 of the 2020 Chinese Pharmacopoeia Ⅳ; the content was determined by using Agilent TC-C_(18) column(4.6 mm×250 mm, 5 μm) for gradient elution, with acetonitrile(A)-0.5% acetic acid solution(B) as the mobile phase; the column temperature was at 30 ℃; the flow rate was 1.0 mL·min~(-1), the detection wavelength was 285 nm; and the injection volume was 10 μL. Compared with Chuanxiong Rhizoma, the extracts of processed products all increased significantly; by the degree of increase, the order was stir-frying Chuanxiong Rhizoma with honey>stir-frying Chuanxiong Rhizoma with rice wine>stir-frying Chuanxiong Rhizoma with Angelicae Dahuricae Radix decoction>stir-frying Chuanxiong Rhizoma with tea decoction; the HPLC method was convenient and reliable, with a high linear relationship of chlorogenic acid, ferulic acid, senkyunolide Ⅰ, coniferyl ferulate, senkyunolide A and ligustilide, and a high precision, repeatability, stability and the sample recovery rate in Chuanxiong Rhizoma and its processed products. There were 15 chromatographic peaks before and after processing, eight of them were identified. Compared with the pre-processing, two chromatographic peaks were added after the stir-frying with honey and rice wine; and four chromatographic peaks were added after the processing with Angelicae Dahuricae Radix decoction; the contents of chlorogenic acid, ferulic acid, senkyunolide Ⅰ, coniferyl ferulate, senkyunolide A, and ligustilide in stir-frying Chuanxiong Rhizoma with rice wine were all reduced. Except for the content of ferulic acid that increased, the content of the other five components decreased in stir-frying Chuanxiong Rhizoma with honey, stir-frying Chuanxiong Rhizoma with tea decoction, and stir-frying Chuanxiong Rhizoma with Angelicae Dahuricae Radix decoction. Rice wine, honey, decoction of tea and Angelicae Dahuricae Radix could all promote the dissolution of chemical components in Chuanxiong Rhizoma, and increase the content of extract; the changes in the contents of six components of different processed products could provide a certain basis for studying chemical composition and efficacy of different processed products of Chuanxiong Rhizoma.
Chlorogenic Acid ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal/analysis* ; Rhizome/chemistry* ; Wine

OBJECTIVETo observe the ethyl carbamate concentrations in different commercial fermented foods in Hangzhou in 2010.

METHODSIn 2010, 237 commercial fermented food samples of eight categories, including yellow wine, white spirit, wine, beer, cooking wine, sauce, vinegar and fermented bean curd, were purchased from 3 different size markets respectively in Hangzhou. The ethyl carbamate was measured by gas chromatography-mass spectrometry in selection ion mode, after the samples were coupled with D5-ethyl carbamate, and purified by diatomite solid phase extraction column.

RESULTSThe results showed that ethyl carbamate was detected in all samples analyzed (100%) with the range from 2.0 µg/kg to 515.0 µg/kg. The ethyl carbamate average (median) levels in 8 food categories were descending with fermented red bean curd (182.2 µg/kg (161.2 µg/kg)), yellow wine (159.6 µg/kg (121.0 µg/kg)), cooking wine (86.8 µg/kg (95.6 µg/kg)), white spirit (72.0 µg/kg (60.5 µg/kg)), soy sauce (47.2 µg/kg (40.7µg/kg)), vinegar (26.7 µg/kg (31.8 µg/kg)), wine (15.7 µg/kg (16.8 µg/kg)) and beer (2.2 µg/kg (2.3 µg/kg)).

CONCLUSIONThe ethyl carbamate was detected in all fermented foods in Hangzhou in 2010, and the levels of ethyl carbamate in red bean curd and yellow wine were higher than others.

Acetic Acid ; analysis ; Alcoholic Beverages ; analysis ; Beer ; analysis ; China ; Fermentation ; Food Analysis ; Food Contamination ; analysis ; Food Inspection ; Gas Chromatography-Mass Spectrometry ; methods ; Urethane ; analysis ; Wine ; analysis

OBJECTIVETo apply the near infrared spectroscopy in quality control for excipients of traditional Chinese medicine (TCM).

METHODA new type of transmittance and reflectance integration sphere accessory and a transmittance accessory were used to collect the spectra of processed honey and rice wine, respectively. Determination method of reducing sugar and ethanol in processed honey were established with partial least squares (PLS).

RESULTThe correlation coefficients (r), the root mean square error of calibration (RMSEC) and the root mean square error of prediction (RMSEP) of the proposed models were 0.9593, 1.00% and 1.19% for reducing sugar; 0.9529, 0.17% and 0.24% for ethanol.

CONCLUSIONThe proposed method is fast, non-destructive, simple and accurate, and can be applied to at-spot detection,

Excipients ; chemistry ; Honey ; analysis ; Medicine, Chinese Traditional ; Oryza ; chemistry ; Quality Control ; Spectroscopy, Near-Infrared ; methods ; Wine ; analysis

OBJECTIVETo explore the effect of processing on the contents of saccharides in Huangqi.

METHODThe contents of reducing saccharides, water-soluble saccharides and poly saccharides in Huangqi and its processed products were determined with phenol-H2SO4 method.

RESULTThe contents of poly saccharides in the alcohol-broiled product were the highest of all the products. The others were all higher than those in the crude drug.

CONCLUSIONDifferent processing methods result in different effects on the above saccharides, which administers to the interpretation of the theory of Huangqi processing.

Astragalus membranaceus ; chemistry ; Drug Stability ; Drugs, Chinese Herbal ; analysis ; Hot Temperature ; Oryza ; Plant Roots ; chemistry ; Plants, Medicinal ; chemistry ; Polysaccharides ; analysis ; Salts ; Technology, Pharmaceutical ; methods ; Wine

OBJECTIVE: For the purpose of more accurate and rapid analysis of aconitine in medicine wine, a reversed-phase High Performance Liquid Chromatography (HPLC) method was developed. METHODS: Standard aconitine was added to the blank wine when the wine sample was pretreated. The pretreatment method of samples, the linear range, the precision, the recoveries in the plasma were investigated by using of white wine plasma spiked with standard aconitine. RESULTS: The linear range was 0.45 approximately 9.0 microg x mL(-1), r=0.998 8. The detective limit was 0.45 microg x mL(-1), The intra and inter-day precision of assay for aconitine were less than 3.1% and 4.7% (n=5) in wine respectively. The recoveries of aconitine were more (97.3+/-2.8)% in medicine wine. The HPLC method has been used to investigate the concentration of aconitine in one forensic medicine case. CONCLUSION The HPLC method of quantitative analysis aconitine is rapid and sensitive. It is only in the 2.0 h that determination of aconitine in the medicine wine.
Aconitine/analysis* ; Chromatography, High Pressure Liquid/methods* ; Forensic Medicine ; Humans ; Male ; Middle Aged ; Quality Control ; Sensitivity and Specificity ; Time Factors ; Wine/analysis*

AIM: To apply an integrated quality assessment strategy to investigate the quality of multiple Chinese commercial dry red wine samples. METHOD: A comprehensive method was developed by combining a high performance liquid chromatography-diode array detector-chemiluminescence (HPLC-DAD-CL) online hyphenated system with an HPLC-ESI-MS technique. RESULTS: Chromatographic and H2O2-scavenging active fingerprints of thirteen batches of different, commercially available Chinese dry red wine samples were obtained and analyzed. Twenty-five compounds, including eighteen antioxidants were identified and evaluated. The dominant and characteristic antioxidants in the samples were identified. The relationships between antioxidant potency and the cultivated variety of grape, producing area, cellaring period, and trade mark are also discussed. CONCLUSION The results provide the feasibility for an integrated quality assessment strategy to be efficiently and objectively used in quality (especially antioxidant activity) assessment and identification of dry red wine.
Antioxidants ; chemistry ; Automation ; instrumentation ; methods ; Chromatography, High Pressure Liquid ; instrumentation ; methods ; Quality Control ; Spectrometry, Mass, Electrospray Ionization ; methods ; Wine ; analysis ; economics ; standards