Effect of sulfur fumigation on quality and safety of Lilii Bulbus / 中国中药杂志

Lilii Bulbus is a commonly used Chinese herbal medicine with both medicinal and edible values, while the market products usually has the problem of sulfur fumigation. Therefore, the quality and safety of Lilii Bulbus products deserve attention. In this study, ultra-high performance liquid chromatography-time of flight-tandem mass spectrometry(UPLC-Q-TOF-MS/MS) was combined with principal component analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA) to analyze the differential components of Lilii Bulbus before and after sulfur fumigation. We identified ten markers generated after sulfur fumigation, summarized their mass fragmentation and transformation patterns, and verified the structures of phenylacrylic acid markers of sulfur fumigation. At the same time, the cytotoxicity of the aqueous extracts of Lilii Bulbus before and after sulfur fumigation was evaluated. The results showed that in the concentration range of 0-800 mg·L~(-1), the aqueous extract of Lilii Bulbus after sulfur fumigation had no significant effect on the viability of human liver LO2 cells, human renal proximal tubular HK-2 cells, and rat adrenal pheochromocytoma PC-12 cells. Moreover, the viability of the cells exposed to the aqueous extract of Lilii Bulbus before and after sulfur fumigation showed no significant difference. This study identified phenylacrylic acid and furostanol saponins as markers of sulfur-fumigated Lilii Bulbus for the first time, and made clear that proper sulfur fumigation of Lilii Bulbus would not produce cytotoxicity, providing a theoretical basis for the rapid identification and quality and safety control of sulfur-fumigated Lilii Bulbus.

Rapid Identification of Gastrodiae Rhizoma with Different Sulfur Fumigation Levels Based on Ultra-fast Gas Phase Electronic Nose / 中国实验方剂学杂志

ObjectiveIn order to find a fast odor-based method for the identification of sulfur fumigated Gastrodiae Rhizoma， an ultra-fast gas phase electronic nose technology was used to identify the odors of different degrees of sulfur fumigated Gastrodiae Rhizoma decoction pieces. MethodHeracles NEO ultra-fast gas phase electronic nose was employed to collect gas chromatograms of unsulfured and sulfured with different degrees of Gastrodiae Rhizoma decoction pieces， gas chromatograms were performed under programmed temperature （initial temperature of 40 ℃， 0.2 ℃·s-1 to 60 ℃， and then 4 ℃·s-1 to 250 ℃）， the sample volume was 5 mL， the incubation temperature was 65 ℃ and incubation time was 35 min. Kovats retention index and the AroChemBase database were used for qualitative analysis， and stoichiometric analysis was performed on this basis. Principal component analysis （PCA）， discriminant factor analysis （DFA） and partial least squares-discriminant analysis （PLS-DA） models were established to identify the Gastrodiae Rhizoma decoction pieces with different degrees of sulfur fumigation. ResultAccording to the comparative analysis of AroChemBase database， there were significant differences in the odor characteristics of sulfur fumigated and non-sulfur fumigated Gastrodiae Rhizoma， cyclopentane， acetone and heptane might be the odor components to distinguish the degree of sulfur fumigation in Gastrodiae Rhizoma decoction pieces. The identification index of PCA model was 81， the accumulative discriminant index of the discriminating factors was 92.09% in DFA model， the supervisory model interpretation rate of PLS-DA model was 0.963 and the predictive ability parameter was 0.956， indicating that PCA， DFA and PLS-DA models could well distinguish Gastrodiae Rhizoma decoction pieces with different sulfur fumigation degrees. ConclusionHeracles NEO ultra-fast gas phase electronic nose can be used as a rapid method to identify and distinguish Gastrodiae Rhizoma decoction pieces with different levels of sulfur fumigation. Meanwhile， it can provide a rapid， simple and green method and technology for identification of traditional Chinese medicine decoction pieces by sulfur fumigation.

Reaction of Chlorogenic Acid with Sulfite and Its Application in Identification of Sulfur-fumigated Herbs / 中国实验方剂学杂志

Objective: To explore the structure and reaction sites of the reaction products of chlorogenic acid and sodium sulfite,and the chemical changes of chlorogenic acid in Lonicerae Japonicae Flos after sulfur fumigating. Method: Chlorogenic acid was reacted with sodium sulfite under mild conditions. Liquid chromatography-mass spectrometry-ion trap-time-of-flight (LC-MS-IT-TOF) and 1H nuclear magnetic resonance spectroscopy (1H-NMR) detection techniques were used to detect the reaction products,and the sulfur-fumigated and unsulfurized Lonicerae Japonicae Flos water extract was detected by LC-MS-IT-TOF. Result: After analyzing the mass spectrometry data of fragment ion,molecular cleavage and accurate molecular weight,according to the results of nuclear magnetic signals of chemical shift,peak intensity and peak splitting, the products of chlorogenic acid and sodium sulfite were preliminarily identified as chlorogenic acid α,β-unsaturated carbonyl addition product:3-((3-(3,4-dihydroxyphenyl)-2-sulfopropyl)oxy)-1,4,5-trihydroxycyclohexane-1-carboxylic acid or 3-((3-(3,4-dihy droxyphenyl)-3-sulfopropyl)oxy)-1,4,5-trihydroxycyclohexane-1-carboxylic acid,and the same characteristic fragments were detected as the addition product in the sulfur fumigated Lonicerae Japonicae Flos,but not found in the unsulfurized. Conclusion: It is the first time to demonstrate the structure and reaction sites of chlorogenic acid and sulfurous acid reaction products,and detect the chlorogenic acid sulfite addition product in sulfur-fumigated Lonicerae Japonicae Flos. Although it is still unclear how the sulfite addition compound produced by sulphur Lonicerae Japonicae Flos affects the efficacy and toxicological activity of Lonicerae Japonicae Flos,we shall still pay attention to the changes of active ingredients in sulphuric medicinal materials. Besides,this study can also provide reference for the studies of chemical composition changes after sulfuration of traditional Chinese medicine containing α,β-unsaturated carbonyl structure.

Effect of Sulfur Fumigation on Content of Chemical Constituents in Panacis Quinquefolii Radix and Preliminary Study on Its Identification Method / 中国实验方剂学杂志

Objective: To elucidate the effect of sulfur fumigation on the content of chemical composition and quality of Panacis Quinquefolii Radix, and to discuss the identification method of sulfur fumigated Panacis Quinquefolii Radix. Method: The content changes of ginsenoside Rb1, Re, Rg1 in Panacis Quinquefolii Radix were determined by HPLC-DAD before and after sulfur fumigation. The content changes of 11 inorganic elements in Panacis Quinquefolii Radix before and after sulfur fumigation were detected by microwave digestion method and inductively coupled plasma emission spectrometry tandem mass spectrometry (ICP-MS). The quality difference of Panacis Quinquefolii Radix before and after sulfur fumigation was qualitatively distinguished combined with the principal component analysis. Result: Three ginsenosides were well separated and showed good linearity with R2 ≥ 0.999.Before sulfur fumigation, the contents of ginsenoside Rg1, Re and Rb1 in Panacis Quinquefolii Radix were (0.897±0.045), (13.092±0.639), (12.896±0.430) g ·kg-1, respectively. After sulfur fumigation, the contents of these three components in Panacis Quinquefolii Radix were (0.807±0.032), (11.968±0.627), (11.752±0.696) g ·kg-1, respectively. After fumigation, the contents of inorganic elements (Cr, Mn, Co, Cu, As, Se, Ag, Cd, Sb, Pb and Fe) from Panacis Quinquefolii Radix increased in varying degrees. According to the distribution results of three-dimensional (3D) scattered points, sulfur and non-sulfur fumigation products of Panacis Quinquefolii Radix could be effectively distinguished. Conclusion: After sulfur fumigation, the contents of ginsenoside Re and Rb1 in Panacis Quinquefolii Radix decrease significantly, but the contents of 11 inorganic elements increase, suggesting that sulfur fumigation may have a great influence on the quality of Panacis Quinquefolii Radix.

Hepatotoxicity study of sulfur-fumigated Ophiopogonis Radix using high content screening / 中草药

Objective: An efficient method was established using high content screening (HCS) for the hepatotoxicity evaluation of sulfur-fumigated Ophiopogonis Radix. Methods: Cytotoxicity of positive control group, negative control group, Ophiopogonis Radix extracts group and sulfur-fumigated Ophiopogonis Radix extracts group were tested based on HepG2 human hepatoma cells. HCS was applied to detect the cell number, DNA content, level of glutathione (GSH), reactive oxgyen species (ROS), and mitochondrial membrane potential (MMP). Results: Compared with the cells of Ophiopogonis Radix extracts group, GSH of sulfur-fumigated Ophiopogonis Radix extracts decreased significantly at the concentration of 50 mg/mL; The MMP of sulfur-fumigated Ophiopogonis Radix extracts changed signally at the concentration of 12.5 mg/mL. Conclusion: Ophiopogonis Radix showed pontential cytotoxicity after sulfur-fumigated. The hepatotoxicity of sulfur-fumigated Ophiopogonis Radix may be related to mitochondria-mediated apoptosis according to the influence of its MMP from the results.

Effect of Heat Treatment on Contents of Sulfur Dioxide Residue and Sulfur-containing Derivatives in Sulfur-fumigated Codonopsis Radix / 中国实验方剂学杂志

Objective: To evaluate the feasibility of heat-treating de-sulfur method for sulfur-fumigated Codonopsis Radix (CR) by investigating the changes in contents of sulfur dioxide residue and sulfur-containing derivatives after sulfur-fumigation.Method: Qualitative and semi-quantitative characterization of sulfur-containing derivatives was analyzed by ultra-performance liquid chromatography-quadrupole-time of flight-mass spectrometry (UPLC-Q-TOF-MS/MS),and sulfur dioxide residues were determined by acid-base titration method. Then the correlations between sulfur dioxide residues and sulfur-containing derivatives in sulfur-fumigated CR samples with different sulfur-fumigation and heat treatment extents were analyzed.Result: Atractylenolide Ⅱ and atractylenolide Ⅲ sulfur-containing derivatives were identified as major characteristic markers of sulfur fumigated CR. With the increase of sulfur-fumigation time,the content of sulfur dioxide residues was continuously increased,while the content of sulfur-containing derivatives was elevated at the beginning and then reached to a plateau, so there was not necessarily a positive correlation between sulfur dioxide residue and the amount of sulfur derivatives. With the increase of heat-treated time,the content of sulfur dioxide residues was continuously decreased,while the content of sulfur-containing derivatives was decreased first and remained at a high level later. There was no clear correlation between sulfur dioxide residue and sulfur-containing derivatives in different sulfur-fumigated and heat-treating de-sulfur degrees of CR.Conclusion: Heat-treatment could decrease the content of sulfur dioxide residue,but the content of sulfur-containing derivatives still remained at a high level, so heat treatment could not reinstate the inner quality of sulfur-fumigated CR to its non-fumigated ones. Therefore, heat-treating de-sulfur is not a feasible method for the quality assurance of sulfur-fumigated CR.

Investigation on Sulfur-fumigated TCM and Its Decoction Piece of China from 2013 to 2017 and Suggestions on the Limit Standard of Sulfur Dioxide Residue / 中国药房

OBJECTIVE： To investigate the status of sulfur fumigation of TCM and its decoction pieces， and to put forward the suggestions on limit standard of sulfur dioxide residue. METHODS： The information of 374 varieties of TCM and sulfur dioxide residue were collected from the provincial and municipal drug inspection institutions of 27 provinces，municipalities and autonomous regions in China during 2013-2017， and then summarized and analyzed. The average value，median value，maximum value，qualification rate and detection rate of sulfur dioxide residue of 121 varieties with the sample number ≥10 batches were classified and statistically analyzed. RESULTS： This investigation involved 374 varieties of TCM and its decoction pieces， and a total of 13 776 batches of samples. The average content of sulfur dioxide was 242 mg/kg，the median value was 27 mg/kg，and the maximum value was 8 782 mg/kg. The overall qualified rate was 79.7％. According to the results of classified statistics， among the 10 varieties whose limit shall not exceed 400 mg/kg，5 varieties，including Codonopsis pilosula， Radix Trichosanthis， Asparagus cochinchinensis， Pueraria lobata， Achyranthes bidentata， were seriously affected by sulfur fumigation，and the qualified rate was less than 80％. Among the varieties with the sample number≥30 batches， there was no or very little abuse of sulfur fumigation in 16 varieties， such as Carthamus tinctorius； 19 varieties， such as Eupolyphaga Steleophaga， had excessive sulfur fumigation， but it was not serious； 25 varieties，such as Lonicera japonica，had severe excessive sulfur fumigation. Among the varieties with the sample number of 10-29 batches，33 varieties including Ziziphus jujube seed had no or very little abuse of sulfur fumigation； 8 varieties including Cuscuta chinensis had excessive sulfur fumigation but were not serious； 10 varieties including Pericarpium Trichosanthis had serious excessive sulfur fumigation. CONCLUSIONS： For the varieties with no or very little excessive sulfur fumigation，it is recommended that batch testing should not be carried out and a single list should be made； for the varieties with sulfur fumigation or severe sulfur fumigation， it is suggested to increase the sulfur dioxide residue limit under all varieties in the 2020 edition of Chinese Pharmacopoeia， and set the limit for the varieties with severe sulfur fumigation to be no more than 400 mg/kg，while the limit for the 2025 edition of Chinese Pharmacopoeia can be reduced to no more than 150 mg/kg. Other varieties should retain the provisions of “sulfur dioxide residue of sulfur dioxide medicinal materials and decoction pieces （except for minerals） shall not exceed 150 mg/kg” in the general rules 0212 “for the identification of medicinal materials and decoction pieces” in the 2015 edition of Chinese Pharmacopoeia （part Ⅳ）.

Sulfur dioxide limit standard and residues in Chinese medicinal materials / 中国中药杂志

The traditional sulfur fumigation processing method has been widely used in the initial processing and storage of traditional Chinese medicinal materials due to its economy, efficiency, convenience, high operability and effect on mold and insect prevention. However, excessive sulfur fumigation of traditional Chinese medicinal materials would lead to the changes in chemical compositions, and even endanger human health. This study showed that traditional Chinese medicinal materials were sulfur fumigated directly after being harvested for quick drying, or fumigated after being weted in the storage process for preventing mold and insects. We found that the sulfur dioxide limits for traditional Chinese medicinal materials were stricter than those for foods. Based on the existing limit standards, we obtained the data of sulfur dioxide residues for 35 types of traditional Chinese medicinal materials in a total of 862 batches. According to the limit standard in the Chinese Pharmacopoeia (150， 400 mg·kg⁻¹), the average over-standard rate of sulfur dioxide was as high as 52.43%, but it was reduced to 29.47% if calculated based on the limit for vegetable additive standard (500 mg·kg⁻¹). Sulfur fumigation issue shall be considered correctly: sulfur dioxide is a type of low toxic substance and less dangerous than aflatoxin and other highly toxic substances, and a small amount of residue would not increase the toxicity of traditional Chinese medicinal materials. However, sulfur fumigation might change the content of chemical substances and affect the quality of traditional Chinese medicinal materials. Furthermore, the exposure hazards of toxic substances are comprehensively correlated with exposure cycle, exposure frequency, and application method. In conclusion, it is suggested to strengthen the studies on the limit standard of traditional Chinese medicinal materials, formulate practical and feasible limit standard for sulfur dioxide residues in traditional Chinese medicinal materials that are consistent with the medication characteristics of traditional Chinese medicinal materials and can guarantee people's demand for safe medication.

Quantitative analysis and stability of -hydroxybenzyl hydrogen sulfite in sulfur-fumigated Gastrodiae Rhizoma / 中国中药杂志

Studies on the characteristic chemical markers of sulfur fumigation have become an effective auxiliary way for quality control of traditional Chinese medicine. This study established a quantitative analysis method for the determination of -hydroxybenzyl hydrogen sulfite (-HS) in Gastrodiae Rhizoma (GR) based on UPLC-MS/MS. Then, 37 batches of GR were screened, and the results showed that 27 batches of them were sulfur-fumigated. Especially, the GR samples in Yunnan producing areas were sulfur-fumigated more seriously. Based on the stability of -HS after different storage time and heat treatment methods, it was found that the content of -HS was stable and reliable in the storage period of 8 months and under normal heat treatment (50, 60, 70, 80 °C) conditions. In conclusion, this study shows a high sensitivity, good selectivity and good stability of -HS, which can provide reference for the quality control and sulfur fumigation screening of GR.

Quality changes in Gastrodia Rhizoma of different origins and forms before and after sulfur fumigation / 中国中药杂志

As Gastrodiae Rhizoma (GR) is one of the herbs more seriously affected by sulfur fumigation, so its quality has been always of a great concern. In this paper, GR samples collected from eight main producing areas and in three forms were fumigated with sulfur and quantitatively and qualitatively analyzed based on UPLC-Q-TOF-MS/MS. The results showed that the contents of gastrodin, parishin, parishin B and parishin C were decreased, while the content of parishin E was increased after sulfur fumigation treatment. Besides, a new sulfur marker named p-hydroxybenzyl hydrogen sulfite was produced in sulfur-fumigated GR samples. As compared with producing origins, forms had a greater impact on the quality of GR, especially in Hongtianma and Wutianma. Besides, the contents of gastrodins and parishins in Hongtianma from Jilin were lowest as compared with those in other producing areas. This might be correlated with planting patterns and environmental factors. In conclusion, sulfur fumigation has a more obvious impact on the quality of GR than origins and forms, which is attributed to the generation of new sulfur fumigated markers.

Changes of chemical compositions and sulfur dioxide residues of Gastrodiae Rhizoma with different storage times / 中国中药杂志

To study the effect of different storage time on the chemical compositions and sulfur dioxide residues of sulfur-fumigated Gastrodiae Rhizoma (GR), and provide scientific basis for solving the quality and safety issues of sulfur-fumigated traditional Chinese medicinal materials. GR, sulfur-fumigated GR and its medicinal slices were stored under the same conditions, and then 8 active ingredients and sulfur dioxide residues were measured respectively. The results showed that the content of gastrodins in sulfur-fumigated GR and its medicinal slices was significantly lower than that in the non-fumigated GR. Moreover, the content of sulfur dioxide residue in sulfur-fumigated GR was significantly higher than that in its medicinal slices. That is to say, sulfur fumigation degree had significantly higher effect on GR quality as compared with its medicinal slices. During the whole storage time (8 months), the content of the eight chemical components in GR was not changed greatly in general. However, after the storage for 4 months, the content of 8 components and sulfur dioxide residues in all of GR samples were significantly changed. In particular, the content of sulfur dioxide residue in GR medicinal materials decreased up to 50% or more.

Optimization of processing technology for sulfur smoked Ophiopogon japonicus based on changes in chemical composition / 中草药

Objective: To optimize the suitable technology of Ophiopogon japonicus (OJ) fumigation based on the changes of relative indexes after the different levels of sulfur fuming. Methods: The phenol-sulfuric acid method was used to determine the content of polysaccharide. HPLC-ELSD method was used to determine the contents of Ophiopogon saponins D (OPD) and D' (OPD') with the mobile phase of acetonitrile-water (50:50), drift tube temperature at 40℃, and nitrogen volumetric flow of 2.0 L/min. The fingerprints of OJ were determined by HPLC-UV method, the mobile phase was eluted with acetonitrile-0.1% phosphoric acid gradient, and the detection wavelength was 297 nm. The contents of ethylophiopogonanones A (MA) and B (MB) were determined using the same method. Using the contents of total polysaccharides of OJ, OPD and OPD', MA and MB, and the contents of other components in the fingerprints as control indexes, and the dosage of sulfur and the time of sulfur fumigation as factors, the central composite design-response surface methodology (CCD-RSM) was used to optimize sulfur fumigation process. Results: In the experimental design range, the content of polysaccharides increased first and then decreased with the increase of sulfur dosage and sulfur fumigation time, and the contents of OPD and OPD' increased slightly and then decreased. The contents of MA and MB were slightly reduced. The sulfur fuming process was determined as follows: sulfur dosage was 120-200 g/m3, sulfur fuming time was 0.6-1.5 h, binomial equation: Y = 0.574 + 0.054 3 X1-0.008 13 X2-0.518 X12 + 0.131X22 + 0.153 X1X2 (R-Sq = 0.971). Process validation: the absolute value of deviation was less than 3%. Conclusion: In this study, the changes of chemical composition of OJ were studied, and the sulfur smelting process suitable for OJ was established.

Influence of sulfur-fumigation on pharmacokinetic of peimine and peiminine of Fritillaria thunbergii in rat / 中草药

Objective: To study the influence of sulfur-fumigation on pharmacokinetic of peimine and peiminine of Fritillaria thunbergii in rat plasma by LC-MS/MS. Methods: After random grouping, 18 SD rats were given the solution of fresh-cut and sulfur-fumigated F. thunbergii by ig administration. The blood drug concentration of peimine and peiminine in rat plasma was determined by HPLC-MS/MS, and the pharmacokinetic parameters were calculated with 3P97 software. Results: The pharmacokinetic parameters of peimine and peiminine of sulfur-fumigated F. thunbergii in rat plasma were (66.40 ± 4.65), (146.72 ± 10.88) ng/mL for Cmax, and (181.79 ± 7.85), (457.38 ± 58.81) ng∙h/mL for AUC, respectively. Those of fresh-cut sample in rat plasma were (186.37 ± 18.8), (227.65 ± 7.01) ng/mL for Cmax, and (197.70 ± 18.69), (566.16 ± 41.55) ng∙h/mL for AUC, respectively. The pharmacokinetic parameters of perimine and peiminine of sulfur-fumigated sample in rat plasma were less than those of fresh-cut sample. Conclusion: The results showed that sulfur-fumigation decreased the bioavailability of peimine and peiminine. This study could provide a basis for further clarifying the influence of sulfur-fumigation on efficacy material base of F.thunbergii.

Chemical markers for quality control of sulfur-fumigated Paeoniae Radix Alba dispensing granules / 中草药

Objective Previous studies found that characteristic sulfur-containing derivatives induced by sulfur-fumigation of medicinal herbs could be used together with sulfur dioxide (SO2) as chemical markers for the quality control of sulfur-fumigated herbs owing to the more specific and reproducibility of characteristic sulfur-containing derivatives over SO2 index. In this paper, the feasibility of these two indices used for the quality control of herbal dispensing granules was further investigated. Methods Using Paeoniae Radix Alba (PRA) as an example, the contents of SO2, paeoniflorin as well as paeoniflorin sulfonate, the characteristic sulfur-containing derivatives of sulfur-fumigated RPA in PRA processing pieces, decoctions, concentrates, and dried extracts were quantified by SO2 residue determination method documented in Chinese Pharmacopeia and HPLC technique, and the transfer ratios of these components during preparation procedures of PRA dispensing granules were evaluated. Results It was found that SO2, paeoniflorin and paeoniflorin sulfonate could all be detectable in the samples of decoctions, concentrates and dried extracts, indicating that these three components could be used as chemical markers to indicate the quality changes during preparation of PRA dispensing granules. However, the transfer ratios of these three components were different from each other, with the contents of SO2 and paeoniflorin decreased, whereas that of paeoniflorin sulfonate increased during preparation of PRA dispensing granules. In addition, in those commercial PRA dispensing granules samples SO2 detectable, paeoniflorin sulfonate also detectable. Conclusion Since SO2 residue is a safety index, while paeoniflorin and paeoniflorin sulfonate can reflect the inner quality and the impact extent of sulfur-fumigation on the quality of PRA dispensing granules respectively, the three components might be used together as chemical markers for the quality control, and consequently to ensure the safety and efficacy of PRA dispensing granules.

Effects of Sulfur Fumigation on Intestinal Absorption of Chrysanthemum Flos / 中国药学杂志

OBJECTIVE: In previous studies, it was found that sulfur fumigation had a destructive effect on chemical constituents of Chrysanthemum Flos. To explore the intestinal absorption of Chrysanthemum Flos after sulfur fumigated. METHODS: The everted rat intestinal sacs were used, and the absorbed was analyzed constituents by UPLC-QTof-MS and HPLC. RESULTS: For sulfur fumigated Chrysanthemum Flos, the contents of flavonoid glycosides were declined in intestinal absorption, while the contents of flavonoid aglycones were not obviously increased. CONCLUSION: Sulphur fumigation lead to the changes of Chrysanthemum Flos, which affects its intestinal absorption.

A new approach for identification of medicinal almonds by fourier transform infrared spectroscopy and systematic clustering of characteristic peaks / 中国天然药物

Medicinal almonds have been used for over 2 000 years and its clinical efficacy includes relieving cough and asthma. The domestic market in China is flooded with different kinds of dried almonds, such as bitter almond (Armeniacae Semen Amarum, AAS), sweet almond (Armeniacae Semen Dulce, ADS), salted almond (Armeniacae Semen Salsa, ASS), and their sulfur-fumigating products (Armeniacae Semen Sulphur Fumabat, ASFS). Wide varieties of almonds may lead to uncertain efficacy, aberrant quality, and even increased safety risk. However, the authentication method for medicinal almonds has not been reported, although imposters may lead to ineffective medical response. In the present study, Fourier transform infrared spectroscopy (FTIR) and the 2-dimensional infrared (2D-IR) spectroscopy were used to identify different almonds, which were extracted with different solvents including water, methanol, ethanol, chloroform and ethyl acetate, respectively. A new simple FTIR method was developed in the present study. According to the gradient solvent polarity, a new 2D IR method was first developed, and the commodities of almonds in China were analyzed by using the FTIR spectroscopy supported by hierarchical clustering of characteristic peaks. Moreover, 5-hydroxymethyl-2-furfural could be used as a detection index and control target in the quality control of medicinal almonds.

Sulfur-containing derivatives as characteristic chemical markers in control of sulfur-fumigated Moutan Cortex / 药学学报

The amount of sulfur dioxide residue is currently employed by Chinese Pharmacopoeia (CP) as an index to screen sulfur-fumigated herbs, but it is unclear if this index can objectively reflect the quality of sulfur-fumigated herbs. In the present study, sulfur-containing derivatives were confirmed in sulfur-fumigated Moutan Cortex (MC) by UPLC-QTOF-MS/MS analysis, and the contents of sulfur-containing derivatives and sulfur dioxide residues were statistically analyzed both in self-made and commercially available sulfur-fumigated and non-fumigated MC as well as the samples thereof before and after eight-month storage. The amount of sulfur dioxide was significantly decreased, but that of the newly-generated sulfur-containing markers was not, after eight-month storage of the sulfur-fumigated MC samples, indicating that the amount of sulfur dioxide residue may not be positively correlated with the quality of sulfur-fumigated MC. Therefore, sulfur dioxide residue index alone may not objectively reflect the sulfur-fumigation extent (quality change extent) of MC, more specific method using characteristic sulfur-containing derivatives as chemical markers should be developed to supplement the sulfur dioxide residue determination in the quality control of sulfur-fumigated MC.

Effects of sulfur fumigation on the quality of Chinese medicinal herbs and the alternative technologies:research advances / 国际药学研究杂志

Sulfur fumigation is a traditional processing method in Chinese herbal medicine,with the effects of being insecti?cide and mildew proof and conducive to storage. Because of the low cost and the convenience in operation,sulfur fumigation has been abused in post harvest handling of herbs in recent years. In this paper,we discuss the effects of sulfur fumigation on the quality of Chi?nese herbal medicine,including the characteristics,chemical composition,heavy metals,trace elements and pharmacological activi?ties,and summarize the progress in several alternative technologies for sulfur fumigation,so as to provide a reliable basis for regula?tions and further research on sulfur fumigation and its alternative technologies.

Effects of sulfur fumigation on the quality of Chinese medicinal herbs and the alternative technologies: Research advances / 国际药学研究杂志

Sulfur fumigation is a traditional processing method in Chinese herbal medicine, with the effects of being insecti⁃cide and mildew proof and conducive to storage. Because of the low cost and the convenience in operation, sulfur fumigation has been abused in post harvest handling of herbs in recent years. In this paper, we discuss the effects of sulfur fumigation on the quality of Chinese herbal medicine, including the characteristics, chemical composition, heavy metals, trace elements and pharmacological activities, and summarize the progress in several alternative technologies for sulfur fumigation, so as to provide a reliable basis for regulations and further research on sulfur fumigation and its alternative technologies.

Comparison of sulfur fumigation processing and direct hot air heating technology on puerarin contents and efficacy of Puerariae Thomsonii Radix / 中国中药杂志

In order to compare the effect of sulfur fumigation processing and direct hot air heating technology on puerarin contents and efficacy of Puerariae Thomsonii Radix, the fresh roots of Pueraria thomsonii were cut into small pieces and prepared into direct sunshine drying samples, direct hot air drying samples, and sulfur fumigation-hot air drying samples. Moisture contents of the samples were then determined. The puerarin contents of different samples were compared by HPLC method. Moreover, the models of drunkenness mice were established, and then with superoxide dismutase (SOD) content as the index, aqueous decoction extracts of Puerariae Thomsonii Radix samples with sulfur fumigation processing and non-sulfur fumigation processing methods were administrated by ig; the effects of sulfur fumigation on contents of SOD in mice liver and serum were determined, and the sulfur fumigation samples and non-sulfur fumigation samples were investigated for moth and mildew under different packaging and storage conditions. Results showed that the sulfur fumigation samples significantly changed the puerarin content from Puerariae Thomsonii Radix. The content of puerarin was decreased gradually when increasing the times of sulfur fumigation and amount of sulfur. SOD content in drunken mice liver and serum was significantly decreased when increasing the times of sulfur fumigation, showing significant difference with both direct sunshine drying group and direct hot air drying group. Moth and mildew were not found in the sulfur fumigation samples and direct hot air drying samples whose moisture contents were lower than the limit in Pharmacopoeia. Research showed that sulfur fumigation can significantly reduce the content of main active ingredients and reduce the efficacy of Puerariae Thomsonii Radix, indicating that the quality of Puerariae Thomsonii Radix was significantly decreased after sulfur fumigation. However, the contents of the main active ingredients, efficacy and storage results of the direct hot air drying samples were similar to those in direct sunshine drying samples, so the hot air drying process was a nice drying technology which could be promoted for use.