Identification of Dalbergia odorifera and Its Counterfeits by HS-GC-MS / 中国实验方剂学杂志

ObjectiveTo screen the differential markers by analyzing volatile components in Dalbergia odorifera and its counterfeits， in order to provide reference for authentication of D. odorifera. MethodThe volatile components in D. odorifera and its counterfeits were detected by headspace gas chromatography-mass spectrometry（HS-GC-MS）， and the GC conditions were heated by procedure（the initial temperature of the column was 50 ℃， the retention time was 1 min， and then the temperature was raised to 300 ℃ at 10 ℃ for 10 min）， the carrier gas was helium， and the flow rate was 1.0 mL·min-1， the split ratio was 10∶1， and the injection volume was 1 mL. The MS conditions used electron bombardment ionization（EI） with the scanning range of m/z 35-550. The compound species were identified by database matching， the relative content of each component was calculated by the peak area normalization method， and principal component analysis（PCA）， orthogonal partial least squares-discrimination analysis（OPLS-DA） and cluster analysis were performed on the detection results by SIMCA 14.1 software， and the differential components of D. odorifera and its counterfeits were screened out according to the variable importance in the projection（VIP） value>2 and P<0.05. ResultA total of 26， 17， 8， 22， 24 and 7 volatile components were identified from D. odorifera， D. bariensis， D. latifolia， D. benthamii， D. pinnata and D. cochinchinensis， respectively. Among them， there were 11 unique volatile components of D. odorifera， 6 unique volatile components of D. bariensis， 3 unique volatile components of D. latifolia， 6 unique volatile components of D. benthamii， 8 unique volatile components of D. pinnata， 4 unique volatile components of D. cochinchinensis. The PCA results showed that， except for D. latifolia and D. cochinchinensis， which could not be clearly distinguished， D. odorifera and other counterfeits could be distributed in a certain area， respectively. The OPLS-DA results showed that D. odorifera and its five counterfeits were clustered into one group each， indicating significant differences in volatile components between D. odorifera and its counterfeits. Finally， a total of 31 differential markers of volatile components between D. odoriferae and its counterfeits were screened. ConclusionHS-GC-MS combined with SIMCA 14.1 software can systematically elucidate the volatile differential components between D. odorifera and its counterfeits， which is suitable for rapid identification of them.

Analysis of Effect of Characteristic Processing with Rice-washed Water on Volatile Components in Raw and Bran-fried Products of Atractylodis Macrocephalae Rhizoma by HS-GC-MS / 中国实验方剂学杂志

ObjectiveBy comparing the differences in composition and content of volatile components between Atractylodis Macrocephalae Rhizoma（AMR）and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR， the effect of processing with rice-washed water on the volatile components in AMR and bran-fried AMR were investigated. MethodHeadspace gas chromatography-mass spectrometry（HS-GC-MS）was used to determine the volatile components in raw products， bran-fried products and their processed products with rice-washed water. GC conditions were programmed temperature（starting temperature of 50 ℃， rising to 140 ℃ at 10 ℃·min-1， maintained for 5 min， then rising to 210 ℃ at 4 ℃·min-1）， splitting ratio of 10∶1， high purity helium as the carrier gas and a solvent delay time of 3 min. MS conditions were an electron bombardment ion source（EI） with an electron collision energy of 70 eV， ion source temperature of 230 ℃， and the detection range of m/z 20-650. The relative contents of the components were determined by the peak area normalization method， the obtained sample data were subjected to principal component analysis（PCA） and orthogonal partial least squares-discriminant analysis（OPLS-DA） by SIMCA 14.1 software， and the differential components of AMR and bleaching AMR， and bran-fried AMR and bran-fried bleaching AMR were screened according to variable importance in the projection（VIP） value>1 and P<0.05. ResultA total of 71 volatile components were identified， including 53 in AMR， 50 in bleaching AMR， 51 in bran-fried AMR， and 44 in bran-fried bleaching AMR. OPLS-DA results showed that there were significant differences between AMR and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR， but not between AMR samples from different origins. The compound composition of AMR and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR did not change， but the contents of monoterpenes and sesquiterpenes changed significantly. ConclusionSignificant changes in the contents of volatile components were observed in AMR and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR， among them， 1，2-dimethyl-4-methylidenecyclopentene， 9，10-dehydro-isolongifolene， γ-elemene， zingiberene， atractylone， silphinene， modhephene and （1S，4S，4aS）-1-isopropyl-4，7-dimethyl-1，2，3，4，4a，5-hexahydronaphthalene can be used as candidate differential markers of volatile components of AMR before and after processing with rice-washed water.

Effect of Jianchangbang Braising Method on Formation of Odor of Polygoni Multiflori Radix Based on HS-GC-MS / 中国实验方剂学杂志

ObjectiveBy comparing the difference of volatile components of the decoction pieces before and after being processed by braising method of Jianchangbang and steaming method included in the 2020 edition of Chinese Pharmacopoeia， the influence of processing methods on the flavor formation of Polygoni Multiflori Radix （PMR） was compared. MethodHeadspace-gas chromatography-mass spectrometry （HS-GC-MS） was used to detect the volatile components of 30 batches of PMR samples from 3 origins with 3 processing methods. The GC was performed under programmed temperature （starting temperature of 40 ℃， rising to 150 ℃ at 5 ℃·min-1， and then rising to 195 ℃ at 10 ℃·min-1） with high purity helium as carrier gas and the split ratio of 10∶1. Mass spectrometry conditions were electron impact ion source （EI） and the detection range of m/z 50-650， the peak area normalization method was used to calculate the relative mass fraction of each component. The chromaticity values of different processed products were measured by a precision colorimeter， the relationship between chromaticity values and relative contents of volatile components was investigated by OriginPro 2021， principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA） were performed on the sample data by SIMCA14.1. The differential components of different processed products of PMR were screened according to the principle of variable importance in the projection （VIP） value>1.5， and the material basis of different odor formation of PMR and its processed products was explored. ResultA total of 59 volatile components were identified， among which 34 were raw products， 33 were braised products， and 27 were steamed products. PCA and OPLS-DA results showed that there were significant differences between the three， but there was no significant difference between samples from different origins of the same processing method. Color parameters of a*， b*， E*ab had no significant correlation with contents of volatile components， while L* was negatively correlated with contents of 2-methyl-2-butenal， 2-methyltetrahydrofuran-3-one and 2，3-dihydro-3，5-dihydroxy-6-methyl-4（H）-pyran-4-one （P<0.05）. The contents of pungent odor components such as caproic acid， nonanoic acid and synthetic camphor decreased after processing， while the contents of sweet flavor components such as 2-methyl-2-butenal， furfural and 5-hydroxymethylfurfural increased after processing， and the contents of furfural， 5-methyl-2-furanmethanol， 5-hydroxymethylfurfural and other aroma components in the braised products were significantly higher than that in the steamed products. ConclusionHS-GC-MS can quickly identify the volatile substance basis that causes the different odors of PMR and its processed products. The effect of processing methods on the odor is greater than that of origin. There is a significant correlation between the color parameter of L* and contents of volatile components， the "raw" taste of PMR may be related to volatile components such as caproic acid， pelargonic acid and synthetic camphor， the "flavor" after processing may be related to the increase of the contents of 2-methyl-2-butenal， furfural， 5-hydroxymethylfurfural， methyl maltol and furfuryl alcohol.

Analysis of Differences of Volatile Components in Atractylodis Rhizoma Before and After Processing with Rice-washed Water by HS-GC-MS / 中国实验方剂学杂志

ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water， the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry （HS-GC-MS） was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea， and their processed products of rice-washed water. Chromatographic conditions were programmed temperature （starting temperature of 50 ℃ for 2 min， rising to 120 ℃ with the speed of 10 ℃·min-1， then rising to 170 ℃ at 2.5 ℃·min-1， and rising to 240 ℃ at 10 ℃·min-1 for 3 min）， the inlet temperature was 280 ℃， the split ratio was 10∶1， and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization （EI） with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis （PCA） and supervised orthogonal partial least squares-discriminant analysis （OPLS-DA） on each sample data， the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection （VIP） value>1. ResultA total of 60 components were identified， among which 40 were rhizomes of A. chinensis and 38 were its processed products， 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively， indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water， and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same， but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids， and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water， the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed， and pinene， 3-carene， p-cymene， ocimene， terpinolene， atractylon， acetic acid and furfural can be used as difference markers before and after processing.

Analysis of Differences of Volatile Components in Atractylodis Rhizoma Before and After Processing with Rice-washed Water by HS-GC-MS / 中国实验方剂学杂志

ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water， the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry （HS-GC-MS） was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea， and their processed products of rice-washed water. Chromatographic conditions were programmed temperature （starting temperature of 50 ℃ for 2 min， rising to 120 ℃ with the speed of 10 ℃·min-1， then rising to 170 ℃ at 2.5 ℃·min-1， and rising to 240 ℃ at 10 ℃·min-1 for 3 min）， the inlet temperature was 280 ℃， the split ratio was 10∶1， and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization （EI） with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis （PCA） and supervised orthogonal partial least squares-discriminant analysis （OPLS-DA） on each sample data， the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection （VIP） value>1. ResultA total of 60 components were identified， among which 40 were rhizomes of A. chinensis and 38 were its processed products， 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively， indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water， and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same， but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids， and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water， the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed， and pinene， 3-carene， p-cymene， ocimene， terpinolene， atractylon， acetic acid and furfural can be used as difference markers before and after processing.

High-speed identification of odor changes and substance basis of Myristicae Semen mildew by electronic nose and HS-GC-MS / 中国中药杂志

This study adopted headspace-gas chromatography-mass spectrometry(HS-GC-MS) and electronic nose to detect volatile components from Myristicae Semen samples with varying degrees of mildew, aiming at rapidly identifying odor changes and substance basis of Myristicae Semen mildew. The experimental data were analyzed by electronic nose and principal component analysis(PCA). The results showed that Myristicae Semen samples were divided into the following three categories by electronic nose and PCA: mildew-free samples, slightly mildewy samples, and mildewy samples. Myristicae Semen samples with different degrees of mildew greatly varied in volatile components. The volatile components in the samples were qualitatively and quantitatively detected by HS-GC-MS, and 59 compounds were obtained. There were significant differences in the composition and content in Myristicae Semen samples with different degrees of mildew. The PCA results were the same as those by electronic nose. Among them, 3-crene, D-limonene, and other terpenes were important indicators for the identification of mildew. Bicyclo[3.1.0]hexane, 4-methylene-1-(1-methylethyl)-, terpinen-4-ol, and other alcohols were key substances to distinguish the degree of mildew. In the later stage of mildew, Myristicae Semen produced a small amount of hydroxyl and aldehyde compounds such as acetaldehyde, 2-methyl-propionaldehyde, 2-methyl-butyraldehyde, and formic acid, which were deduced as the material basis of the mildew. The results are expected to provide a basis for the rapid identification of Myristicae Semen with different degrees of mildew, odor changes, and the substance basis of mildew.

Study on Material Basis and Processing Principle of Fishy Smell of Pheretima aspergillum by Electronic Nose and HS-GC-MS / 中国实验方剂学杂志

Objective:To analyze and compare the fishy components in raw, stir-fried, liquorice-processed, vinegar-processed and wine-processed products of Pheretima aspergillum, and explore the material basis and processing principle of fishy smell of P. aspergillum. Method:Heracles Ⅱ ultra-fasted gas chromatography electronic nose technology combined with chemometrics was used for the overall analysis of volatile components in raw P. aspergillum and its processed products. Headspace gas chromatography-mass spectrometry (HS-GC-MS) was used to analyze and identify the volatile compositions in the raw products and processed products. Gas chromatographic conditions were as following：temperature program (initial temperature at 60 ℃, kept for 5 min, up to 120 ℃ with the heating rate of 3 ℃·min-1, and then up to 230 ℃ with the heating rate of 10 ℃·min-1 and finished), the inlet temperature at 280 ℃, high purity helium as the carrier gas, the flow rate of 1.0 mL·min-1, the split ratio of 20∶1. Mass spectrum conditions were as following：electron impact ionization (EI), electron collision energy of 70 eV, ion source temperature of 230 ℃, quadrupole temperature at 150 ℃, scanning range of m/z 50-550. The relative content of each component was calculated by peak area normalization. Result:Principal component analysis (PCA) and discriminant factor analysis (DFA) of the electronic nose showed that the raw products and its processed products could be clearly distinguished from each other. Among them, the difference between raw products and stir-fried, liquorice-processed products was small, but the difference between raw products and vinegar-processed, wine-processed products was large. A total of 25, 27, 22, 26 and 33 components were respectively identified from raw, stir-fried, liquorice-processed, vinegar-processed and wine-processed products of P. aspergillum, there were 13 common components in these products, including 4 aldehydes (isovaleraldehyde, 2-methylbutyraldehyde, hexanal, benzaldehyde), 2 ketones (2-heptanone, 2-tridecanone), 1 carboxylic acid (lauric acid), 4 heterocyclic compounds (2-methylpyrazine, 2,5-dimethyl pyrazine, 2-pentylfuran, 2-ethyl-6-methyl pyrazine), 1 amine (trimethylamine) and 1 alcohol (1-octen-3-ol). Conclusion:The odorous components in the raw products are mainly derived from aldehydes (isovaleraldehyde, 2-methylbutyraldehyde, isobutyraldehyde, 2-ethylhexanal, hexanal) and amines (trimethylamine). Odorous components of P. aspergillum can be reduced effectively by stir-fried and liquorice, vinegar, wine processing, while flavoring substances can be increased by wine processing to cover its ugly odor. This paper can provide scientific basis for the deodorization of P. aspergillum by processing, and also provide reference for the analysis and correction of ugly odor of other animal medicines.

Comparative study on differences of resin-containing drugs in Dracaena from different appearance based on HS-GC-MS and chemometrics / 中国中药杂志

Resin-containing drugs in Dracaena from four different appearances were analyzed by headspace sampling-gas chromatography-mass spectrometry(HS-GC-MS) metabolomics technique and hierarchical clustering analysis(HCA) chemometrics method. This study was to analyze differential volatile components in resin-containing drugs in Dracaena from different appearance and metabolic pathways. The results of partial least squares discriminant analysis(PLS-DA) and HCA analysis indicated that there was little difference in volatile components between fiber-rich sample and hollow cork cambium sample, however, the volatile components in the two samples compared with whole body resin-containing sample and resin-secreting aggregated sample had a large metabolic difference. Twenty differential metabolites were screened by VIP and P values of PLS-DA. The content of these differential metabolites was significantly higher in whole body resin-containing sample and resin-secreting aggregated sample than in fiber-rich sample and hollow cork cambium sample. Sixteen significant metabolic pathways were obtained through enrichment analysis(P<0.05), mainly involved in terpenoids biosynthesis and phenylpropanoid metabolism. This result provided a reference for further study of resin formation mechanism of resin-containing drugs in Dracaena from different appearances. At the same time, it also provided a reference for establishing a multi-index quality evaluation system.

Measuring eleven kinds of chlorobenzenes and hexachlorobutadiene in drinking water by HS-GC / 上海预防医学

Objective To apply the HS-GC method to measure eleven kinds of chlorobenzenes and hexachlorobutadiene in drinking water . Methods We put 10 mL water sample into a 20 mL vial containing 2.5 g sodium chloride .The vial was stirred at 80℃ for 15 mins prior to headspace sampling . Eleven kinds of chlorobenzenes were separated completely by Rtx-1 701 capillary column(30.00 m ×0.25 mm ×0.25 μm),detected by electron capture detectors . Results The linearity of the method ranged from 1.00-32.00 μg/L, 0.20-6.40 μg/L, 0.05-1.60 μg/L, 0.02-0.64 μg/L, 0.02-0.64 μg/L and 0 .01-0 .32 μg/L for dichlorobenzene isomers , trichlorobenzene isomers , tetrachlorobenzene isomers , pentachlorobenzene , hexachlorobenzene and hexachlorobutadiene .In case of a 10 mL water sample , the lowest detected range of mass concentration was 0.001 62-0.262 00 μg/L.The additional standard recovery rate of finished water samples was in the range of 80%-119%with the relative standard deviation (RSD) in the range of 2.24%-4.99%. Conclusion This method is simple, fast, sensitive and needs no organic solvents .It is suitable for measuring both chlorobenzene compounds and hexachlorobutadiene in drinking water simultaneously .

Analysis of volatile components from Actinidia valvata by HS-GC-MS based on retention index / 药学实践杂志

Objective To establish a method for determining volatile components from Actinidia valvata Dunn .Methods A static headspace‐gas chromatography‐mass spectrometry (HS‐GC‐MS) method was used to analyze volatile components , and the separated peaks were identified by mass spectal library searching combined with retention index comparison .Results 42 volatile components were separated from Actinidia valvata Dunn and 25 of them were identified ,mainly including alcohols ,es‐ters ,aldehydes ,hydrocarbons and so on .Conclusion Combined with retention index calculation ,this method improved accuracy of qualitation of HS‐GC‐MS and provided scientific proof for the exploitation and utilization of Actinidia valvata Dunn .

Evaluation of uncertainty in determination of ethanol in human blood by auto HS-GC with internal standard curve method / 中国法医学杂志

ObjectiveTo evaluate the uncertainty for the determination of ethanol in human blood by auto-headspace gas chromatography (HS-GC) with internal standard curve method.Methods Each source of uncertainty, arising from the procedure of testing, was analyzed and conifrmed according to the guidelines of the uncertainty in measurement . After each uncertainty component was quantized, the combined standard uncertainty and the expanded uncertainty of the result were calculated.Results The relative uncertainty brought from the measurement repeatability, standard solution of the ethanol, the sample of blood, internal standard solution of the tert-butyl alcohol, the calibration cure, gas chromatography were 3.4%,0.71%,0.61%,0.41%,1.1% and 1.3% respectively; the relative expanded uncertainty of ethanol in blood was 3.9%.Conclusion The measurement uncertainty of the concentration of ethanol was came primarily from the measurement repeatability of sample, HS-GC and standard curve of ethanol.

Simultaneous Determination of Vinyl Chloride and Vinylidene Chloride in Drug Packaging Materials Con-taining Polyvinyl Chloride/Polyvinylidene Chloride by HS-GC / 中国药师

Objective:To develop a method for the simultaneous determination of vinyl chloride and vinylidenechloride in drug packaging materials containing polyvinyl chloride /polyvinylidene chloride by HS-GC.Methods: A Stabilwax (30.0 m ×0.25 mm, 0.25 μm) capillary column and an FID detector were adopted .The headspace equivalent temperature was 80℃for 30 min and the col-umn temperature was 40℃.The inlet temperature was 190℃and the detector temperature was 210℃.N2 was used as the carrier gas . The flow rate was 1.0 ml · min-1 .Results: Vinyl chloride had a good linear relationship within the range of 0.5-2.5 μg ( r =0.996 7), and the average recovery was 90.4%(RSD=0.9%, n=9).Vinylidenechloride had a good linear relationship within the range of 1.0-5.0 μg (r=0.999 0), and the average recovery was 90.0%(RSD=0.6%, n=9).Conclusion: The method is fast and accurate in the simultaneous determination of vinyl chloride and vinylidenechloride in drug packaging materials containing polyvinyl chloride/polyvinylidene chloride .

Content Determination of Menthol in 56 Batches of Qiangli Pipa Syrup by HS-GC / 中国药房

OBJECTIVE:To establish the HS-GC method for the content determination of menthol in Qiangli Pipa syrup,and the content of menthol in 56 batches of Qiangli Pipa syrup commercially available was determined. METHODS:HS-GC was per-formed on the column of Agilent HP-INNOWAX,column temperature was 130 ℃(maintaining 7 min),FID was used as detector, inlet temperature was 200 ℃,detector temperature was 250 ℃,carrier gas was high-purity nitrogen,flow rate was 3 ml/min,split ratio was 10∶1 and the injection volume was 1 000 μl. RESULTS:The linear range of menthol was 0.007 07-0.141 40 mg/ml(r=0.999 1);RSDs of precision,reproducibility and stability tests were no more than 3.37%;average recovery was 94.3%-99.6%(RSD=1.86%,n=6). There was significant difference in the contents of menthol in 56 batches Qiangli Pipa syrup. CONCLU-SIONS:The method is simple,sensitive,accurate and reliable,and can be used for content determination of menthol in Qiangli Pi-pa syrup. The sampling results show it is necessary to update the detecting items for the content of Qiangli pipa loquat and strength-en the quality control of it.

Determination of Residual Solvent DMF in Imiquimod by HS-GC / 中国药师

Objective: To establish a new method for determining residual organic solvent DMF in imiquimod. Methods: The samples were injected into an Agilent HP-PLOT/Q capillary column(30 m × 0. 530 mm,40. 0 μm) by a headspace sampler and ana-lyzed with an FID detector, the carrier gas was nitrogen, the inlet temperature was 250℃, and the detector temperature was 270℃. The column temperature was programmed raised. Results: The resolution among the peaks of DMF and the other residual solvents could meet the requirements. There was a good linearity within the experimental concentration range. The average recovery was 94. 6%(RSD=4. 0%, n=9). The limit of quantification and the limit of detection was 4. 809μg·ml-1 and 0. 963μg·ml-1, respectively. Conclusion:The method is convenient, accurate and sensitive, which can be used in the determination of residual solvent DMF in imi-quimod.

Determination of Menthol in Xiao’ er Fufang Mahuangjian Jiegeng Syrups by HS-GC / 中国药师

Objective:To establish an HS-GC method for the determination of menthol in Xiao ’ er Fufang Mahuangjian Jiegeng syrups. Methods:An Agilent DB-WAX column(30 m × 0. 53 mm,1. 0 μm)with an FID detector was used;the inlet temperature was 150℃, the detector temperature was 250℃;the flow rate of the carrier gas ( N2 ) was 2. 0 ml·min-1 , the split ratio was 1∶1; the headspace equilibrium temperature was 80℃, the balance time was 30 min, and the sample volume was 1ml. Results:The calibration curve of menthol was within the range of 2. 09-20. 92 μg·ml-1, which showed a good linear relationship (r=0. 999 1). The average recovery of menthol was 98. 0%(RSD=1. 8%, n=6). Conclusion: The method is simple, accurate and reproducible, and can be used for the determination of menthol in Xiao’ er Fufang Mahuangjian Jiegeng syrups.

Rapid Determination of Methanol and Ethanol in Human Plasma by Head Space Gas Chromatography / 中国药房

OBJECTIVE:To establish a HS-GC method for determining methanol and ethanol in human plasma METHOD_S:An external standard method was used The stationary phase was a glass column packed with GDX-102 The carrier gas was nitrogen The column temperature was 140℃ and both the injector temperature and the detector temperature were 200℃ RE_SULTS:A good linearity was obtained in the range of 0 2～7 5g/L of methanol and ethanol The within-day RSD was less than 4% and the between-day RSD less than 5 5% The recoveries were (100 9?3 8)% for methanol,(101 5?3 4)% for et_hanol,respectively The limits of detection for both methanol and ethanol were less than 0 01g/L CONCLUSION:This method is simple,rapid and precise

Determination of Borneol and Menthol in Compound Shexiang Injection by HS-GC / 中药新药与临床药理

Objective To establish the determination of borneol and menthol in C ompound Shexiang Injection by HS-GC.Methods A Rtx-Wax column (30 m?0.25 mm? 0.25 ?m) and FID were used.The injector and the detector temperature was 260 ℃ .Column temperature was controlled by programming:initial temperature at 140 ℃and holding 2 min,and temperature increase at 10 ℃?min-1,final temperatur e at 220 ℃for 4 min. Results The linear range of borneol and menthol was 13.025 ～416.8 ?g?mL-1 (r=0.999 5,n=6) and 13.125～420 ?g?mL-1 (r=0.999 7,n=6) ,and the average recovery was 98.97 %(RSD=3.0 %,n=6) and 97.65 %(RSD=2.1 % ,n=6),respectively.Conclusion The method is sensitive,accurate and reproduci ble for simultaneous determination of borneol and menthol in Compound Shexiang I njection.

Analysis of the cyanide in biological samples by using HS / 中国法医学杂志

Objective to establish a method used for qualitative and quantitative determination of the cyanide in biological samples by using HS/GC/ECD. Method C1CN was formed as the choramines-T derivative through reaction of the potassium cyanide with chloramines-T and then was analyzed by GC/ ECD/HS. Results if 0.2ug potassium cyanide was added to 1ml blood sample, the recovery was 84.6% and RSD was 6.39%. If 0.5ug potassium cyanide was added to 1. 0g liver, the recovery was 67.3 % and RSD was 5.05%. The detection limit of blood sample was 5ng/ml. Conclusion This method can be used for analyzing the cyanide in biological samples quantitatively.