Comparison on Changes of Volatile Components in Gecko Before and After Processing by HS-SPME-GC-MS / 中国实验方剂学杂志

ObjectiveOn the basis of sensory evaluation， the changes of volatile components in gecko before and after processing were compared， and the odor correction effect of different processing methods of gecko was discussed. MethodRaw products， fried yellow products， vinegar processed products， wine processed products， talcum powder scalding products and white wine sprayed products after scalding talcum powder of gecko were prepared， and 10 odor assessors were invited to evaluate the 6 samples in turn by sensory evaluation. Headspace solid-phase microextraction-gas chromatography-mass spectrometry （HS-SPME-GC-MS） and relative odor activity value （ROAV） were used to analyze the key odor components， and multivariate statistical methods were used to analyze the difference of volatile components between raw and processed products of gecko. Taking water-soluble extract and protein contents as internal indicators， sensory evaluation score and content ranking of differential components as external indicators， and assigning a weight of 0.25 to them respectively， the comprehensive scores of raw products and processed products of gecko were calculated to evaluate the odor correction effect of each processing method. ResultThe average sensory evaluation scores of the raw products， fried yellow products， vinegar processed products， wine processed products， talcum powder scalding products and white wine sprayed products after scalding talcum powder of gecko were 1.6， 5.2， 6.2， 6.1， 7.2 and 8.0， respectively. ROAV results showed that key components affecting odor of gecko were 2-ethyl-3，5-dimethylpyrazine， isovaleraldehyde， trimethylamine， 1-octen-3-ol， n-octanal， nonanal， 2-methylnaphthalene， γ-octanolide， 2-heptanone and phenol. Principal component analysis （PCA） significantly distinguished raw products from processed products. Orthogonal partial least squares-discriminant analysis （OPLS-DA） results showed that there were 16， 13， 16， 16， 16 differential components between raw products， fried yellow products， vinegar processed products， wine processed products， talcum powder scalding products and white wine sprayed products after scalding talcum powder of gecko. Among these differential components， there were 4 common components， namely， the contents of different odor components （2-methylnaphthalene and 2-ethyl-p-xylene） decreased， while the contents of different flavor components （2-decanone and 2，3，5-trimethylpyrazine） increased. The comprehensive scoring results showed that the odor correction effect of each processed products was in the order of talcum powder scalding products>wine processed products>vinegar processed products>fried yellow products>white wine sprayed products after scalding talcum powder. ConclusionTalcum powder scalding is a better method to improve the odor of gecko， and it can provide an experimental basis for the processing of gecko to correct the odor.

Analysis of Quality Changes of Platycladi Semen Before and After Deterioration Based on HS-SPME/GC-MS and Electronic Sensory Technology / 中国实验方剂学杂志

ObjectiveTo analyze the quality changes of Platycladi Semen before and after the deterioration of moth-eaten and rancidity during storage. MethodFour types samples of Platycladi Semen， including normal， moth-eaten， oxidative rancidity and hydrolytic rancidity， were determined for volatile components， odor， and taste based on headspace solid phase microextraction/gas chromatography-mass spectrometry （HS-SPME/GC-MS） and electronic sensory techniques such as electronic nose and electronic tongue. Volatile components were identified by searching the database and manual comparison， the odor and taste were determined by the response values of the electronic nose and electronic tongue sensors， and the difference between samples before and after deterioration was studied by multivariate statistical analysis. ResultA total of 85 compounds were identified in Platycladi Semen samples. Compared with the normal samples， the number of volatile compounds in samples after hydrolytic rancidity decreased by 5， the number of volatile compounds in samples after moth-eaten and oxidative rancidity increased by 1 and 21， respectively. Aldehydes and acids accounted for majority of types. Among them， the contents of N-hexanoic acid， hexanal and propionic acid in the samples of oxidative rancidity reached 11.49%， 10.21% and 7.52%， which became the key indicators of rancidity. There was significant variance among the odor components corresponding to W1W， W2W and W1S sensors by electronic nose analysis. It was indicated that the value of sourness in deteriorated samples generally increased by mean of electronic tongue analysis. Compared with normal samples， the moth-eaten samples had changed slightly and rancidity samples had changed significantly especially oxidative rancidity samples of volatile components， odor and taste by multivariate statistical analysis. ConclusionIn terms of Platycladi Semen， the oxidative rancidity caused by nature storage for 12 months has the greatest impact on the quality. Therefore， it should be mainly to prevent oxidative rancidity to ensure the quality of Platycladi Semen.

Establishment and Application of Identification Method for Fishy Odor of Cordyceps Based on HS-SPME/GC-QQQ-MS/MS / 中国实验方剂学杂志

Objective:To establish and apply a new practical analytical method for identifying the fishy odor of Cordyceps based on headspace-solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry （HS-SPME/GC-QQQ-MS/MS） technique. Method:The InertCap Pure-WAX capillary column （0.25 mm×30 m， 0.25 μm） was used for chromatographic separation. The injection port temperature was set at 250 ℃. The injection mode was split injection with a ratio of 5∶1. High purity helium was used as the carrier gas and control mode was set to constant pressure. The column flow rate was 1.43 mL∙min^-1， the linear velocity was 43.3 cm∙s^-1， and the purge flow rate was 3.0 mL∙min^-1. The chromatographic column temperature program as follows：maintained the initial temperature at 50 ℃ for 5 min， and increased the temperature at a rate of 10 ℃∙min^-1 to 250 ℃， held for 10 min. The column equilibrium time was 2.0 min. The ion source of mass spectrographic analysis was electron ionization with ion source temperature of 200 ℃， and the monitoring mode was set to multiple reaction monitoring. Result:Seven batches of Cordyceps samples were collected， including 3 batches from Sichuan， 3 batches from Qinghai and 1 batch from Tibet. There were six batches of counterfeits， including 3 batches from Sichuan， 2 batches from Guizhou and 1 batch in Xinjiang. A total of 81 volatile compounds were screened out in Cordyceps， which could be divided into 13 types （esters， ketones， aldehydes and others） according to the compound structure， indicating that the fishy odor of Cordyceps was a complex odor. There was no significant difference in the types of volatile compounds of Cordyceps from different regions， which suggested that these volatile compounds in Cordyceps produced in Tibet （Naqu）， Qinghai （Yushu and Guoluo） and Sichuan （Litang， Rangtang and Seda） were relatively consistent. However， the contents of some volatile compounds in Cordyceps produced in different regions were quite different， and 16 volatile compounds with significant difference were screened out， including 1-methoxy-2-propyl acetate， <italic>γ</italic>-octalactone， hexyl acetate and others， those compounds maybe could been used as the quality markers for identification of regions of Cordyceps. There was a large difference in volatile compounds between Cordyceps and its counterfeits， and 34 volatile compounds were screened out， including ethyl acetate， acetophenone， 2-ethyl-1-hexanol and others， those compounds maybe could been used as the quality markers for authenticity identification of Cordyceps. Conclusion:In summary， the established method for identifying the fishy odor of Cordyceps in this paper has the characteristics of high sensitivity， accuracy and simplicity， which can provide reference for the analysis of volatile compounds in other Chinese herbal medicines.

Volatile compounds in off-odor honey / Compostos voláteis em mel com odor indesejável

ABSTRACT: Climatic conditions in the mid-northern region of Mato Grosso State in Brazil are favorable for beekeeping. However, since 2011, the honey production chain has suffered losses because the production of off-odor honey has made it impossible to market the honey. Reports from beekeepers indicated a relationship between the off-odor in the honey and the nectar of Borreria verticillata (L.) G. Mey (Rubiaceae). In this study, the botanical origins and volatile profiles of ten off-odor honeys (H1-H10) and flowers of B. verticillata were evaluated. Palynological and sensorial analyses of the honeys were performed; a scale from 1 to 4 was applied for the sensorial analysis, in which 1 indicates no off-odor and 4 indicates extreme off-odor. Analysis of volatile was performed by using headspace solid-phase microextraction and gas chromatography-mass spectroscopy methods. The honeys investigated were classified with very high to intense off-odors, except H4 and H5, which did not differ from the control honey (no off-odor). Palynological analyses showed that honeys H1-H4, H7, and H9 were monofloral from B. verticillata, whereas in H5, H6, H8, and H10 this pollen were accessory. However, there was no quantitative correlation between the B. verticillata pollen content and the off-odor attributes of the honeys. Skatole was identified in all of the honeys except H4, H5, and the control honeys, suggesting that skatole contributed to the off-odor attributes of the products. However, further studies are required to investigate the origin of the skatole because it is not transferred directly from B. verticillata flowers to the honey.

RESUMO: As condições climáticas da região Centro-Norte do Estado de Mato Grosso são favoráveis a apicultura, contudo ocorrem prejuízos nesta cadeia produtiva desde 2011 devido a produção de mel com odor indesejável, o que impossibilitou sua comercialização. Relatos dos apicultores apontaram relação da ocorrência do odor indesejável no mel com o néctar Borreria verticillata (L.) G. Mey (Rubiaceae). Neste estudo foi avaliado a origem botânica e o perfil de voláteis de méis (M1 até M10) com odor indesejável e das flores de B. verticillata. Foi realizada a análise polínica do mel e também sensorial, empregando-se uma escala de um a quatro pontos, em que um refere-se a nenhum odor desagradável e quatro, extremo odor desagradável. A análise de compostos voláteis no mel e nas flores de B. verticillata foi realizada utilizando microextração em fase sólida por headspace e cromatografia gasosa acoplada a detector por espectrometria de massas. Os méis investigados foram classificados desde muito a extremo odor desagradável, exceto os méis M4 e M5, que não diferiram do mel controle (sem odor indesejável). Os méis M1 até M4, M7 e M9 eram monoflorais de B. verticillata, enquanto M5, M6, M8 e M10 o pólen B. verticillata era acessório. Todavia, não foi observada correlação quantitativa entre o teor deste pólen e o atributo odor indesejável. O escatol foi identificado nos méis investigados, exceto em M4, M5 e mel controle. Estes resultados sugerem que o escatol contribuiu para o atributo odor desagradável do produto. Contudo, mais estudos devem ser conduzidos para investigar a origem do odor indesejável, porque o escatol não foi transferido diretamente das flores para o mel.

Antagonistic activity of volatile metabolites from Trichoderma asperellum / 生物工程学报

Trichoderma spp. is a kind of filamentous fungi with important biocontrol value. Twelve strains of Trichoderma spp. were isolated from the soils of different types of crops in Shaoxing, Zhejiang and Foshan, Guangdong. The antagonistic resistance to Fusarium oxysporum was compared by plate confrontation test. The further analysis of volatile secondary metabolites for two strains were carried out using HS-SPME-GC-MS analysis. The results showed that T. asperellum ZJSX5003 and GDFS1009 had fast growth ability, and the inhibition effects on F. oxysporum were 73% and 74% respectively. Six identical volatile metabolites were detected as follows 2-Methyl-1-propanol, 3-Methyl-1-butanol, 3-Methyl-3-buten-1-ol, Acetyl methyl carbinol, Butane-2,3-diol and 6-n-pentyl-2H-pyran-2-one (6-PAP). Among them, 6-PAP was validated to have a higher inhibitory effect on F. oxysporum in vitro. This study will provide basis for the development of biocontrol agents with metabolites of Trichoderma, such as 6-PAP.

Analysis and identification of volatile constituents in different parts of Murrayae Folium et Cacumen by HS-SPME-GC-MS / 国际药学研究杂志

Objective: To analyze,identify and compare the volatile components in different medicinal parts of Murrayae Folium et Cacumen(Kamuning). Methods: The volatile components were extracted by headspace solid-phase microextraction(HS-SPME)and analyzed by gas chromatography-mass spectrometry(GC-MS). The relative contents were calculated for each of the volatile components by the area normalization method. Results A total of 74 compounds were identified in the root,stem and leaf of Murrayae Folium et Cacumen,among which there were 8 components in common in the three parts,and the numbers of specific components in roots,stems and leaves were 23,27 and 32,respectively. Conclu- sion The present HS-SPME-GC-MS method was suitable for the analysis of volatile components in the different parts of Murrayae Folium et Cacumen. Some volatile components were identified to be medicinal ingredients. The present results provide a reference for further development and application of the Murrayae Folium et Cacumen resources.

Comparison of Volatile Oil of Domestic and Foreign Panacix Quinquefolii Radix by HS-SPME/GC-MS / 中国实验方剂学杂志

Objective: To determine the volatile chemical constituents of Panacix Quinquefolii Radix of different origins and different growth years,in order to provide the theoretical basis for the further development and utilization of Panacix Quinquefolii Radix. Method: Headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) was used to extract,analyze and identify the volatile constituents of Panacix Quinquefolii Radix. The chromatographic peak area normalization method was used to determine the relative amount of ingredients. Result: A total of 151 compounds were identified in Panacix Quinquefolii Radix samples,including 99 hydrocarbons,21 alcohol phenols,7 aldehydes,8 ketones,1 ester,15 heterocyclics and other compounds. Totally 68 kinds of compounds were identified in the roots of three-year-old Jilin Baishan,and the mass fraction accounted for 98.27%,67 compounds were identified in the roots of four-year-old Jilin Baishan,and the mass fraction accounted for 98.79%,65 compounds were identified in 3-year-old Panacix Quinquefolii Radix root,and the mass fraction accounted for 95.81%,and 63 compounds were identified in 4-year-old Panacix Quinquefolii Radix root,and the mass fraction accounted for 99.67%. The specific components of the volatile oil components of the four Panacix Quinquefolii Radix samples were 24,23,19,and 23,respectively,and the total composition was 16 species. Conclusion: The content and composition of volatile chemical constituents of Panacix Quinquefolii Radix of different origins are very different. This experiment provides a reference for the future quality evaluation of Panacix Quinquefolii Radix medicinal materials,rational development and utilization of resources.

Analysis on Odorous Components in Different Processed Products of Periplaneta americana by HS-SPME-GC-MS / 中国实验方剂学杂志

Objective:To analyze the odorous components and their contents in raw products, wine-processed products, vinegar-processed products and wheat bran-processed products of Periplaneta americana. Method:Headspace solid-phase microextraction (HS-SPME) was used to extract the volatile components from different processed products, the chemical compositions were analyzed by gas chromatography-mass spectrometry (GC-MS), and the relative contents of each component was calculated by peak area normalization method. Result:A total of 41, 32, 40 and 47 components were respectively identified from raw, wine-processed, vinegar-processed and wheat bran-processed products of P. americana, involving a total of 13 common components. Conclusion:The odorous components in the raw products are mainly derived from aldehydes, alcohols, amines, hydrocarbons and other volatile substances. Odorous components can be reduced effectively and flavoring substances can be increased by wine, vinegar and wheat bran processing. This study provides a scientific basis for the further study of correcting odor of P. americana, it also provides a reference for analysis and correction of odor of animal medicines.

Determination of cyclohexanol in urine by headspace solid-phase microextraction coupled with gas chromatography / 中华劳动卫生职业病杂志

Objective@#To establish a method for determining cyclohexanol in urine by headspace solid-phase microextraction (HS/SPME) coupled with gas chromatography (GC) .@*Methods@#After the urine sample was hydrolyzed by β-glucuronidase, 2.0 g of NaCl was added, then the analyte in urine was adsorbed by a CAR/PDMS solid phase micro-extraction head in a water bath at 50 ℃ for 20 min. And the extraction head was inserted into the gas chromatograph gasification chamber to desorb, the analyte was detected after separated by the capillary through the flame ionization detector.@*Results@#The linear range of the method was 0.1-5.0 mg/L with the correlation coefficients (r) 0.999. The average recovery was 84.5%-96.3%, the inter-day precision was 3.81%-6.00%, and the detection limit was 0.03 mg/L.@*Conclusion@#The method is founded to be low detection limit, simple operation and no need of organic solvent. So it is suitable for the detection of cyclohexanol in urine of occupational exposure to cyclohexanone.

A comparative analysis of volatile components of moxa cone and stick from different manufacturers using HS-SPME-GC-MS / 国际药学研究杂志

Objective: To analyze the volatile components in different brands of moxa cones and sticks. Methods: Head- space solid-phase microextraction coupled with gas chromatography-mass spectrometry(HS-SPME-GC-MS)was used to qualitatively analyze volatile components in different brands of moxa cones and sticks. The relative content of each component was calculated by peak area normalization method. The experimental data were comprehensively evaluated by principal component analysis. Results: The total ion chromatograms of the volatile components of moxa cones and sticks in 7 batches produced by 5 manufacturers were simi- lar on the whole,but the volatile components were still different. Eighty-six compounds were identified initially. The most common components were found to be eucalyptol,camphor,terpineol,bornyl acetate,caryophyllene,caryophyllene,oxide(-)-4-terpineol, and cliff ketone. Conclusion: Using HS-SPME-GC-MS could quickly provide information for the chemical composition of the volatile componentsin themoxaconesandsticks,andtherearesignificantdifferencesin thevolatilecomponentsamongdifferentbrands.

Comparison of volatile components in Schisandra propinqua from different habitats by HS-SPME-GC-MS / 中国中药杂志

A headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) method was developed and optimized for qualitative and semi quantitative analysis of volatile components from Schisandra propinqua, a kind of Yi Nationality herb medicine. This method was used for analysis and evaluation of volatile components from S.propinqua from four different geometrical origins (Yunnan Wuding, Yunnan Luoping, Guizhou Qingzhen and Hubei Shennongjia). 51, 53, 52， 50 compounds were identified from the above four kinds of samples respectively, in which 46 volatile components were contained in all of these four origins. The volatile components in these samples from different geographical origins were then compared by using principal component analysis, cluster analysis and other chemometrics methods. The results suggested that the analysis of volatile components can be used to distinguish the S.propinqua from four origins, and those samples from close geographical origins were more similar in volatile components. The developed method was stable, reliable, and suitable for rapid analysis of volatile components from S.propinqua, providing reference for quality control, drug development and scientific utilization of the herb.

Analysis of Volatile Ingredients of Ligusticum chuanxiong before and after Processed with Wine by Head-space Solid Phase Microextraction-GC/MS / 中国药房

OBJECTIVE:To compare the differences in the volatile ingredients of raw products and wine processed products of Ligusticum chuanxiong,and provide reference for its pharmacological activity research and clinical application. METHODS:Head-space solid phase microextraction-GC/MS was used to analyze the volatile components of L. chuanxiong before and after processed with wine. And area normalization method was adopted to calculate the relative percentage content of each component. RESULTS:28 components were isolated from the raw products and 24 components were identified,accounting for 99.70% of total volatile components. 2-methyl-2,3-dihydro-1H-inden-2-ol(20.06%),α-selinene(17.97%)and 4-ethyl-3-nonen-5-yne(9.24%)were high-er in contents. 21 components were isolated from the wine processed products and 18 components were identified,accounting for 89.74% of total volatile components. 4-ethyl-nonen-5-yne (12.97%) was the highest in content,followed by 4-carene (11.74%) and α-selinene(10.79%). Compared with raw products,the contents of active components α-pinene and β-elemene were increased. CONCLUSIONS:The volatile components and their relative contents of L. chuanxiong before and after processed with wine show certain differences,and volatile components after wine processed are relatively reduced. However,contents of the components with analgesic effect are increased,and its analgesic effect is superior to raw products.

Analysis of the similarities and differences of volatile components of dalbergiae odoriferae lignum and its adulterants / 国际药学研究杂志

Objective To analyze similarities and differences of volatile components of Dalbergiae Odoriferae Lignum (DOL) and its adulterants, so as to provide a scientific basis for the identification of the authenticity of the pros and cons of DOL, and offer the reference for die further study of DOL. Methods With headspace solid phase microextraetion (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS), volatile components of DOL and its adulterants were analyzed and identified, and the relative content of each component was calculated by area normalization method. Results There were 70 compounds detected, in which 38 compounds were identified. They were mainly alkenes, alcohols, aldehydes and ketones. A total of 42 compounds were detected from DOL volatile components, and 25 components were identified, accounting for 96.54% of the volatile components; 28 peaks were detected from its adulterants, and 19 compounds were identified, accounting for 80.7% of the volatile components. Conclusion There were huge differences in volatile components between DOL and its adulterants. Only 6 common components were defected both in the DOL and it’s adulterants, with their quite different contents. The main component of DOL was nerolidol, accounting for 61.47% of volatile components; the main component of its adulterants was beta selinene, accounting for 59.04% of total volatile components. The present result provides a scientific guidance for the identification of true or false DOL and also a reference for the further development of Dalbergia wood.

Analysis of the similarities and differences of volatile components of Dalbergiae Odoriferae Lignum and its adulterants / 国际药学研究杂志

Objective To analyze similarities and differences of volatile components of Dalbergiae Odoriferae Lignum(DOL) and its adulterants,so as to provide a scientific basis for the identification of the authenticity of the pros and cons of DOL,and offer the reference for the further study of DOL. Methods With headspace solid phase microextraction(HS-SPME)combined with gas chromatography-mass spectrometry(GC-MS),volatile components of DOL and its adulterants were analyzed and identified,and the relative content of each component was calculated by area normalization method. Results There were 70 compounds detected,in which 38 compounds were identified. They were mainly alkenes,alcohols,aldehydes and ketones. A total of 42 compounds were de?tected from DOL volatile components,and 25 components were identified,accounting for 96.54% of the volatile components;28 peaks were detected from its adulterants,and 19 compounds were identified,accounting for 80.7%of the volatile components. Con?clusion There were huge differences in volatile components between DOL and its adulterants. Only 6 common components were de?fected both in the DOL and it's adulterants,with their quite different contents. The main component of DOL was nerolidol,accounting for 61.47%of volatile components;the main component of its adulterants was beta selinene,accounting for 59.04%of total volatile components. The present result provides a scientific guidance for the identification of true or false DOL and also a reference for the fur?ther development of Dalbergia wood.

Analysis of Volatile Ingredients of Ligusticum chuanxiong before and after Processed with Wine by Head-space Solid Phase Microextraction-GC/MS / 中国药房

OBJECTIVE:To compare the differences in the volatile ingredients of raw products and wine processed products of Ligusticum chuanxiong,and provide reference for its pharmacological activity research and clinical application. METHODS:Head-space solid phase microextraction-GC/MS was used to analyze the volatile components of L. chuanxiong before and after processed with wine. And area normalization method was adopted to calculate the relative percentage content of each component. RESULTS:28 components were isolated from the raw products and 24 components were identified,accounting for 99.70% of total volatile components. 2-methyl-2,3-dihydro-1H-inden-2-ol(20.06%),α-selinene(17.97%)and 4-ethyl-3-nonen-5-yne(9.24%)were high-er in contents. 21 components were isolated from the wine processed products and 18 components were identified,accounting for 89.74% of total volatile components. 4-ethyl-nonen-5-yne (12.97%) was the highest in content,followed by 4-carene (11.74%) and α-selinene(10.79%). Compared with raw products,the contents of active components α-pinene and β-elemene were increased. CONCLUSIONS:The volatile components and their relative contents of L. chuanxiong before and after processed with wine show certain differences,and volatile components after wine processed are relatively reduced. However,contents of the components with analgesic effect are increased,and its analgesic effect is superior to raw products.

Quantitative determination of seven major absorbed volatile constituents in mice brain, liver and blood after intragastric administration of Asari Radix et Rhizoma suspension by headspace-solid phase microextraction-gas chromatography-mass spectrometry / 中国中药杂志

A headspace-solid phase microextraction-gas chromatography-mass spectrometry method（HS-SPME-GC-MS） was adopted for the quantitative study of 4-allylanisole, methyl eugenol, 2,3,5-trimethoxytoluene, 3,4,5-trimethoxytoluene, sarisan, 3,5-dimethoxytoluene and safrole in mice brain, liver tissues and blood after intragastric administration of Asari Radix et Rhizoma. A VF-WAXms (30 m×0.25 mm, 0.25 μm film thickness) capillary column and SPME fiber coated with 65 μm polydimethylsiloxane/divinylbenzene (PDMS/DVB) were used. The calibration curves of seven volatile constituents were established to validate the method's stability (RSD<15%), repeatability (RSD<9.5%), accuracy (RSD<22%), relative recovery (87.0%-108%) and extraction recovery (74.9%-102%). The validated HS-SPME-GC-MS assay was applied to determine the concentrations of seven constituents in liver, brain and blood. The detected contents were 0.22,0.14 μg•g⁻¹,0.25 mg•L⁻¹ (4-allylanisole), 1.1, 0.39 μg•g⁻¹, 0.69 mg•L⁻¹ (methyl eugenol), 0.45, 0.13 μg•g⁻¹, 0.54 mg•L⁻¹ (2,3,5-trimethoxytoluene), 0.51, 0.15 μg•g⁻¹, 0.45 mg•L⁻¹ (3,4,5-trimethoxytoluene), 0.48, 0.039 μg•g⁻¹, 0.69 mg•L ⁻¹ (sarisan), 2.2, 1.2 μg•g⁻¹, 1.5 mg•L⁻¹ (3,5-dimethoxytoluene) and 1.3, 0.67 μg•g⁻¹, 1.1 mg•L⁻¹ (safrole) respectively. This HS-SPME-GC-MS method is rapid and convenient, with a small sample size, and applicable for the analysis and determination of volatile constituents in traditional Chinese medicines, which provides scientific data for further studies on effective substances and toxic substances in Asari Radix et Rhizoma.

Analysis of Volatile Components in Descurainia sophia and Lepidium apetalum / 中国药房

OBJECTIVE:To analyze the volatile components in Descurainia sophia and Lepidium apetalum and compare its dif-ferences. METHODS:HS-SPME was conducted for extracting volatile components in D. sophia and L. apetalum,GC-MS was used for detecting components,and area normalization method was adopted for calculating relative content of each component. RE-SULTS:The volatile components in D. sophia and L. apetalum were 25 and 18,accounting for 75.76% and 64.29% of total vola-tile components,respectively,and chemical components with the highest contents were β-caryophyllene and O-tolunitrile. CON-CLUSIONS:The method is simple,reliable,and can be used for the analysis of volatile components in D. sophia and L. apetalum. The volatile components show great differences in the kinds and contents,the study can provide basis for rapid identification of D. sophia and L. apetalum.

Comparative Study of Volatile Compounds in Different Parts of Albiziajul Ibrissin Durazz / 中国药师

Objective:To compare and analyze the volatile components in different medicinal parts of silktree Albizzia julibrissin and their relative contents .Methods:Chromatography-mass spectrometry using headspace solid phase microextraction combined with gas method ( HS-SPME-GC-MS) was used to analyze the volatile components in the bark and flowers of silktree Albizzia julibrissin and the relative contents were calculated by a peak area normalization method .Results:In the bark and flowers of silktree Albizzia julibris-sin, totally 30 and 33 compounds were respectively identified , which respectively accounted for 73.20%and 88.29%of the total vola-tile.A total of 15 components, including alkanes, alkenes, aldehydes, furans, alcohols and acids were in the bark and flowers of silk-tree Albizzia julibrissin, among them, the content of cineole was the highest (bark:15.02%and flowers:21.9%).Conclusion:The HS-SPME technique can be used to analyze and compare the volatile components in the bark and flowers of silktree Albizzia julibrissin, which provides scientific basis for the reasonable development and application of the bark and flowers of silktree Albizzia julibrissin.

Determinación de trihalometanos en aguas de consumo humano por microextracción en fase sólida- cromatografía de gases en Pereira, Colombia / Determination of trihalomethanes in drinking water by solid phase microextraction- gas chromatography in Pereira, Colombia / Determinação de trihalometanos na água para consumo humano por microextração em fase sólida -cromatografia em fase gasosa em Pereira, Colômbia

La desinfección del agua con cloro genera subproductos como los trihalometanos (THM´s), a los cuales se les atribuyen propiedades cancerígenas y con efecto adverso en el sistema reproductivo. Se estandarizó un método simple, rápido y libre de solventes fue para la determinación de THM´s en aguas para consumo humano utilizando microextracción en fase sólida con espacio de cabeza combinada con cromatografía de gases con detector de microcaptura de electrones (HS-SPME-GC-µECD). Fueron estudiados y optimizados parámetros experimentales. Las condiciones optimizadas fueron: 20 min de extracción a 37 °C en presencia de 25% de NaCl y con una agitación de 200 rpm; con tiempo de desorción de 4 min a 250 °C. Se determinaron los límites de detección y cuantificación del método y se realizó el análisis de los trihalometanos de 75 muestras de agua de la planta de tratamiento de Aguas y Aguas de la ciudad de Pereira. El rango lineal de 5-100 mg/L fue establecido con una desviación estándar relativa (%RSD) en el rango 6,1-10,1 %. Los límites de detección estuvieron en el rango 3,8-7,8 mg/L. El promedio de la concentración de THM´s fue de 55,5 mg/L.

Water disinfection with chlorine generates byproducts such as trihalomethanes (THM's), to which cancer risk and a potential adverse effect on the reproductive system properties are attributed. The maximum permitted level of THM's in the United States is 80-100 µg/L, while in Colombia it is 200 µg/L. In this study a simple, fast and solvent-free method was developed for the determination of THM's in drinking water using solid phase microextraction in combination with head space gas chromatography microcapture electron detector (HS-SPME-GC-µECD) and used for quantification of THM's in drinking water. Experimental parameters such as extraction time, extraction temperature, desorption temperature, magnetic stirring, and addition of salt were studied. Limits of detection and quantification were determined and the analysis of THM´s in 75 samples of water from the treatment plant of Pereira city were performed. Optimized conditions were 20 min extraction at 37 °C in the presence of 25% NaCl and with stirring at 200 rpm; with a desorption time of 4 min at 250 °C. Linear range of 5-100 µg/L was established with a relative standard deviation (% RSD) in the range 6.1-10.1%. Detection limits ranged from 3.8 to 7.8 µg/L. Average concentration of THMs was 55.5 µg/L which was within International and National requirements.

A desinfecção da água com cloro gera subprodutos como trihalometanos (THM´s), aos quais são atribuídos o risco de câncer e efeitos adversos sobre o sistema reprodutivo. Foi estandardizado um método simples, rápido e livre de solventes para a determinação de THM´s nas águas para consumo humano usando microextração em fase sólida com espaço de cabeça em combinação de cromatografia gasosa com microcaptura de eletrões (HS-SPME-GC-µECD). Foram estudados e otimizados os parâmetros experimentais. As condições optimizadas foram de 20 minutos de extração, a 37 °C na presença de 25% de NaCl, com agitação de 200 rpm e com tempo de dessorção de 4 min a 250 °C. Os limites de detecção e quantificação do método foram determinados e foi realizada a análise de trihalometanos em 75 amostras de água da estação de tratamento da cidade de Pereira. A gama linear de 5-100 mg/L foi estabelecida com um desvio-padrão relativo (%RSD) na gama de 6,1-10,1%. Os limites de detecção foram de 3,8 a 7,8, mg/L. A média de concentração de THM´s foi de 55,5 mg/L.

Determination of Organochlorine Pesticides and Chlorobenzene Compounds in Water by Headspace Solid-Phase Microextraction Combined with Gas Chromatography / 环境与健康杂志

0.99. The recovery rates were 72.25% -109.0% with the relative standard deviation (RSD) of 1.82% -11.61% . Conclusion The method is fast,simple,sensitive and needs no organic solvent and it is applicable to the determination of organochlorine pesticides and chlorobenzene compounds in water.