Determination of camphor residue and borneol content in Qingchang suppository by GC / 药学实践杂志

Objective To establish a gas chromatography for simultaneous determination of camphor residue and borneolum content in Qingchang Suppository. Methods Gas chromatograph method was used. The chromatographic column was Agilent capillary column(30 m×0.25 mm×0.25 µm). The column temperature was 140 ℃. The sample injection temperature was 250 ℃. The FID detector temperature was 250 ℃. Results Camphor，borneol and isoborneol content showed good linear in the extent of 0.0299~1.497(r=1.000), 0.0205~1.025(r=1.000), 0.0097~0.4830 µg (r=1.000). RSDs of precision，stability and repeatability test results were less than 2%. The recovery was 99.7%, 101.0%, 102.5%. Conclusion This method is simple and quick with accurate result, which could be used for the content determination of Borneol in Qingchang Suppository.

Solution of camphor volatility in industrialized preparation of cataplasm based on inclusion technology of HP-β-CD / 中草药

Objective: To reduce or avoid the volatilization loss of camphor (CA) in the industrialized preparation of cataplasm, using the inclusion technology of HP-β-CD. Methods: The HP-β-CD inclusion compound of CA (CA-HP-β-CD) was prepared by the constant temperature stirring method. The preparation processing of CA-HP-β-CD was optimized with inclusion efficiency as an index, and the pharmaceutical properties of CA-HP-β-CD were characterized by DSC, UV and SEM. The CA and CA-HP-β-CD were prepared to cataplasm at the industrial-scale production respectively, then the content of CA was determined and the statistical analysis was carried out. Results: The inclusion efficiency of CA-HP-β-CD for CA was (68.57 ± 1.26)% when the CA-HP-β-CD was prepared with the mass ratio of CA to HP-β-CD 1:3, the working temperature at 35 ℃ and stirring at 300 r/min for 4.0 h. The DSC, UV and SEM scans showed that there was a good compatibility between CA and HP-β-CD, and CA could be fully encapsulated by HP-β-CD and formed a stable inclusion complex of CA-HP-β-CD. Results of industrial-scale production of cataplasm for CA and CA-HP-β-CD revealed that the retention rate (actual content/feeding quantity) were (80.13 ± 1.05)% and (39.45 ± 1.38)%, respectively. And there was a statistically significant difference between them (t-test, P < 0.01), indicating that the HP-β-CD inclusion complex effectively reduce the volatilization loss of camphor CA. Conclusion: The volatilization loss of CA at the industrial-scale production of cataplasm was effectively reduced by the CA-HP-β-CD, which improves the utilization rate of CA and reduces the cost, and provides ideas and reference for the research and development of cataplasm of volatile drugs.

Quackery and Superstitions: The Skin Doctor’s Bane

@#Camphor, a waxy white sublimable chemical, widely used worldwide by various communities for many religious purposes. Here we report a clinical image of self-inflicted injury from burning camphor on the palm resulting in burns. It also highlights the sociocultural pattern of this injury and need of psychopathic and therapeutic help of the patients.

Establishment and application of fingerprint and quantitative method of volatile components in Shuangyu Granules / 中草药

Objective To establish the GC fingerprint and components quantitative determination of Shuangyu Granules (SG) for quality control. Methods Agilent DB-1 capillary column (30 m × 0.32 mm, 0.25 μm) was used with upper column volume of 1 μL and split ratio of 25∶1; Injection port was 230 ℃ and detector temperatures was 250 ℃; The carrier gas was nitrogen and its flow rate was 0.6 mL/min. The column temperature was raised by program. Results The fingerprints with good separation and repeatability included 12 mutual common peaks, and the similarity of each batch was more than 0.95. Seven chemical components were identified by GC/MS and standard compounds, which were eucalyptol (peak 2), camphor (peak 3), menthone (peak 4), borneol (peak 5), menthol (peak 6), pulegone (peak 9), and undecanone (peak 10); Among which, peaks of 1, and 10—12 were from Houttuyniae Herba, peaks of 2 and 5 from Artemisiae Argyi Folium and Menthae Haplocalycis Herba, peak of 3 from Artemisiae Argyi Folium, peak of 4, 6, 8 and 9 from Menthae Haplocalycis Herba, peak of 7 from Menthae Haplocalycis Herba, Artemisiae Argyi Folium and Houttuyniae Herba. Moreover, eucalyptol and menthol were quantified and the average recovery rates of eucalyptol and menthol were 103.9% and 98.2% (RSD were 2.1% and 2.3%), respectively. The content of eucalyptol and menthol in 10 batches samples were 0.17—0.23 mg/g and 0.45—0.67 mg/g, respectively. Conclusion The method of fingerprint and quantitative analysis of two components in SG was rapid, simple, and accurate, which could be used for the quality control of SG.

Simultaneous Determination of Contents of 6 Components in the Oil of Blumea balsamifera by GC / 中国药房

OBJECTIVE： To establish a method for simultaneous determination of contents of β-pinene， linalool， L-camphor， L-borneol， β-caryophyllene and xanthoxylin in the oil of Blumea balsamifera. METHODS： GC method was adopted. The determination was performed on RTX-1701 capillary column （programmed temperature）. The FID detector was controlled at 240 ℃. The inlet temperature was set at 240 ℃. The carrier gas was high-purity nitrogen 3 mL/min. The the sample size was 0.5 μL， and split ratio was 50 ∶ 1. RESULTS： The linear range of β-pinene， linalool， L-camphor， L-borneol， β-caryophyllene and xanthoxylin were 0.029 7-0.267 1 mg/mL （r＝0.999 9）， 0.024 3-0.218 9 mg/mL （r＝0.999 9）， 0.126 0-1.134 0 mg/mL （r＝0.999 9）， 0.217 2-1.954 8 mg/mL （r＝0.999 9）， 0.136 3-1.226 9 mg/mL （r＝0.999 9）， 0.044 5-0.400 3 mg/mL（r＝0.999 5）， respectively. The limits of quantitation were 0.028 5， 0.008 7， 0.018 6， 0.016 8， 0.014 5， 0.042 1 mg/mL； the limits of detection were 0.009 4， 0.002 9， 0.006 1， 0.005 5， 0.004 8， 0.013 9 mg/mL， respectively. RSDs of precision， stability， reproducibility and durability tests were all lower than 3％. The average recoveries were 98.13％-101.30％（RSD＝1.20％，n＝9），98.44％-101.81％（RSD＝1.28％，n＝9），98.26％-101.05％（RSD＝1.19％，n＝9），99.08％-101.58％（RSD＝0.89％，n＝9），98.66％-101.66％（RSD＝1.17％，n＝9），98.84％-103.60％（RSD＝0.96％，n＝9）， respectively. The contents of 6 components in the sample were 14.552-46.766， 16.951-22.096， 80.597-113.115， 205.224-242.537， 47.761-135.697， 26.493-45.771 mg/g， respectively. CONCLUSIONS： The established method is simple， accurate， precise and reproducible， which can be used for simultaneous determination of contents of 6 components in the oil of B. balsamifera. It can provide reference for comprehensive evaluation and extraction technology study of the oil of B. balsamifera.

Limit Test of Camphor in Niuhuang Qingxin Pills (Prescription of the Bureau) / 医药导报

Objective To establish limit test method of camphor in Niuhuang qingxin pills (prescription of the bureau) . Methods The separation was performed on an HP-INNOWAX capillary column (0.25 mm×30 m, 0.25 μm) and the column temperature was 110 ℃ . The temperatures of the inlet and the FID detector were 200 and 230 ℃ , respectively. The flow rate of the carrier gas was 1.8 mL·min-1 and the split ratio was 10:1. The injection volume was 1 μL. Results Good linearity was obtained for camphor within the range of 1.65 to 165 μg·mL-1, and the average recovery of low, medium, high concentration were 99.12％, 99.56％ and 99.56％, respectively,with RSD were 1.01％,0.69％ and 0.38％, respectively. Trace camphor was found in 7 samples out of 38 samples from 9 manufactures. Conclusion The proposed method was accurate, sensitive and simple, and was suitable for quality evaluation and safety control of Niuhuang qingxin pills (prescription of the bureau) .

Simultaneous Determination of Borneol and Camphor in Xingkening Capsules by GC / 中国药师

Objective: To establish a GC method for the determination of borneol and camphor in Xingkening capsules. Methods:A capillary column using polyethylene glycol 20000 (PEG-20M) as the stationary phase (30 m×0. 53 mm,1 μm) was employed. The flow rate of carries gas (N2) was 3. 0 ml·min-1. The inlet temperature was 200℃, the temperature of flame ionization detector was 210℃, the column temperature was 140℃, and the split ratio was 1 ∶ 1. Results: The linear range of borneol was 13. 25-1 325. 19 μg·ml-1(r=0. 999 9), and the average recovery was 100. 22% with the RSD of 0. 92% (n=6). The linear range of camphor was 1. 029-16. 464 μg·ml-1(r=0. 997 5),and the average recovery was 98. 89% with the RSD of 2. 78% (n=6). Conclusion: The method is simple, accurate and reliable, which can be used for the quality control of borneol and camphor in Xingkening capsules.

Applications of GC-MS/MS automated mass spectral deconvolution and multi reaction monitor qualitative and quantitative analysis of volatile components of Chenxiang Huaqi Tablets / 中草药

Objective To analytically screen the volatile components from Chenxiang Huaqi Tablets (CHT) using gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) combined with automated mass spectral deconvolution, and establish the methods of multiple components contents (camphor, bornyl acetate, and patchouli alcohol) from CHT using multi reaction monitor (MRM). Methods The chromatographic column was HP-5MS (30 m × 0.32 mm × 0.25 μm). Temperature program: the initial temperature was 100 ℃, at 15 ℃/min up to 300 ℃ for 2 min. Injection port temperature was 280 ℃; Ionization methods: EI ion source with ion source temperature of 230 ℃; Quadrupole temperature was 150 ℃; Interface temperature was 280 ℃; Inject volume was 1 μl. Results A total of thirteen components were screened by automated mass spectral deconvolution soft. Under the conditions of MRM collection, camphor, bornyl acetate, and patchouli alcohol were in the range of 4.5-90 mg/mL (r = 0.999 8), 3.3-66 mg/mL (r = 0.999 8), and 2.6-51.5 mg/mL (r = 0.999 9), respectively, the ratio of each component concentration to its peak area was linear, and the average recovery (n = 6) was 101.15%, 102.64%, and 100.10% respectively; The mass fraction of 10 batches of samples were in the ranges of 0.278-0.311, 0.381-0.438, and 0.229-0.381. Conclusion The method is accurate, simple, and good repeatability. It can be used for the simultaneous determination of camphor, bornyl acetate, and patchouli alcohol in CHT, which provides a reference for the improvement of the quality of this variety.

Determination of Eucalyptol, Camphor and Menthol in Compound Menthol Camphor Eucalyptus Oil Solution by GC / 中国药师

Objective: To establish a method for the determination of eucalyptol, camphor and menthol in compound menthol camphor eucalyptus oil solution by GC.Methods: An HP-INNOWAX 19091N-216 capillary column(60 m× 0.32 mm , 0.50 μm)was used.The carrier gas was nitrogen with the flow rate of 30 ml·min-1 , the gas was hydrogen with the flow rate of 40 ml·min-1 and the oxidant gas was air with the flow rate of 400 ml· min-1.The detector was FID and the inlet temperature was 250℃.The temperature program was as follows: the initial column temperature was 50℃, and then risen to 160℃ with a rate of 10℃·min-1 and kept for 5 min, and finally risen to 220℃ with a rate of 20℃·min-1 and kept for 3 min.The split ratio was 15∶1 and the injection volume was 1 μl.Results: The linear range of eucalyptol, camphor and menthol was 0.031 9-2.550 0 mg·ml-1 (r=1.000 0), 0.041 3-3.305 0 mg·ml-1 (r=1.000 0) and 0.053 7-4.294 0 mg·ml-1 (r=1.000 0), respectively.The average recovery was 98.24% (RSD=0.3% , n =9), 98.97% (RSD=0.4% , n =9) and 98.98% (RSD=0.5% , n =9), respectively.Conclusion: The method is sensitive and accurate with good stability, which can be used to determine the contents of eucalyptol, camphor and menthol in compound menthol camphor eucalyptus oil solution.

Improvement of quality standards of Arthritis Ointment / 中草药

Objective: To improve the quality standards for Arthritis Ointment. Methods: TLC was applied to identification of Angelica dahurica in qualitative identification. The camphor and borneol contents were determined by GC. Results: The TLC spots of A. dahurica were distinct and reproducible, and negative without interference. The linear ranges of camphor and borneol were 0.401 41-4.014 1 and 0.393 34-3.933 4 μg. The average contents of camphor and borneol were 6.038 0 and 5.353 9 mg/g. The average recoveries of camphor and borneol were 99.32% and 99.82%. Conclusion: The established quality standards are accurate, simple, and feasible, and could be used for quality control of Arthritis Ointment.

Optimization for prescription of Sanqi Traumatic Ointment by Box-Behnken test design and research on its transdermal permeability in vitro / 中草药

Objective To prepare Sanqi Traumatic Ointment (STO) and study its transdermal permeation properties in vitro. Methods In this paper, the appearance description, high-temperature test, low-temperature test and centrifugal test were taken as indexes. Based on the result of a single factor experiment, the formula for the STO was optimized by Box-Behnken test. Franz diffusing cells method was chosen to investigate the tansdermal infiltration capacity of ointment with different mentha camphor penetration enhancers' in vitro, taking dracorhodin, ginsenoside Rg1, asperosaponi VI, and ginsenoside Rb1 as index components. Results The optimal ratio of the prescription was as follows: lauryl sodium sulfate-stearyl alcohol-vaseline (1.61:26.72:27.10). The promoting effect of different concentration of penetration enhancers on dracorhodin, ginsenoside Rg1, ginsenoside VI, and asperosaponin Rb1 penetration were better; The promoting effect of 3% concentration for index component was better, and this preparation had good stability; The transdermal rates of dracorhodin, ginsenoside Rg1, asperosaponi VI, and ginsenoside Rb1 were 3.971, 6.368, 0.415, and 2.780 μg/(cm2∙h).Conclusion STO had a good release and transdermal properties, and transdermal actions were consistent with zero-order kinetics.

Simultaneous determination of dexamethasone acetate , camphor and phenol in compound cream by HPLC method / 药学实践杂志

Objective To establish a HPLC method for simultaneously determining the content of dexamethasone ace-tate ,camphor and phenol in compound cream .Methods The separation was performed on a SHIADZU-GL Inertsil? ODS-3 RP C18 analytical column with the mobile phase consisting of methanol-water (60:40) .The flow rate was 1 .0 ml/min .The detection wave length was 285 nm and the column temperature was 40 ℃ .Results Dexamethasone acetate ,camphor and phe-nol showed good linearity (r> 0 .9995 , n= 7) within the concentration range of 4 .024-40 .24 ,101 .7-2033 and 10 .38-425 .2 μg/ml ,respectively . The average recovery of dexamethasone acetate ,camphor and phenol was 101 .2％ (RSD was 0.56％ ) ,99 .89％ (RSD was 0 .72％ ) ,100 .2％ (RSD was 0 .97％ ) ,respectively .Moreover ,the RSDs were less than 1 .5％ in the repeated tests .Conclusion The method was simple ,quick and accurate .It is suitable for the quality control of dexametha-sone acetate camphor and phenol cream .

Detection Method for Three Ultraviolet Absorbers in Cosmetics / 中国药师

Objective: To develop an HPLC method for the simultaneous determination of 3 ultraviolet absorbers (benzylidene camphor sulfonic acid, camphor benzalkonium methosulfate, 4-methylbenzylidene camphor) in cosmetics.Methods: After extracted by acetonitrile-methanol-ammonium acetate aqueous solution-tetrahydrofur(30∶35∶30∶5, v/v)(for lotion and milk) or acetonitrile-methanol-ammonium acetate aqueous solution(30∶20∶50, v/v)(for cream and powder), the UV absorbers were separated on a Thermo scientific C18 column (250 mm×4.6 mm,5 μm) at 35 ℃ with methanol, acetonitrile and 0.02 mol·L-1ammonium acetate aqueous solution (pH 5.15 adjusted by glacial acetic acid) as the mobile phase with gradient elution at the flow rate of 1.0 ml·min-1, and then analyzed by a DAD detector at the wavelength of 288 nm and 300 nm.Results: Benzylidene camphor sulfonic acid, camphor benzalkonium methosulfate and 4-methylbenzylidene camphor showed good linearity within the range of 12.26-98.06 μg·ml-1(r=0.999 9), 9.31-74.48 μg·ml-1(r=0.999 9) and 6.86-54.88 μg·ml-1(r=0.999 9), respectively.The limit of detection (LOD) and the limit of quantitation (LOQ) were 4.6, 6.4 and 1.6 ng and 17.4, 15.9 and 5.5 ng, respectively.The average recovery was 99.2%(RSD=1.58%), 99.8%(RSD=2.38%) and 99.2%(RSD=2.03%)(n=36), respectively.Conclusion: The method is simple, rapid, reproducible, accurate and reliable, and can be applied in the determination of ultraviolet absorbers in cosmetics.

Clinical application of Depulpin inactivation agent in emergency treatment of acute pulpitis / 实用口腔医学杂志

21 8 patients with acute pulpitis were randomly divided into 2 groups.1 09 cases were treated by Depulpin inactivation agent (group DI)for emergency management,another 1 09 cases were treated by pulp drainage with phenol camphor cotton ball(group CP).The effective analgesia rate of DI and CP group was 95.4% and 69.7% respectively(P<0.001 ).

Preparation of emulsion-hydrogel transdermal patch of essential oil from Artemisiae Argyi Folium and its transdermal characteristics / 中草药

Objective: To optimize formulations of emulsion-hydrogel transdermal patch of essential oil from Artemisia Argyi Folium, and to evaluate its transdermal characteristics in vitro. Methods: The formulations were optimized by orthogonal experiment with four factors including hydrogel patch carrier (sodium polyacrylate NP-700), crosslinking agent (dihydroxyaluminium aminoacetate), crosslinking modifier (EDTA), and moisturizing agent (glycerol). Initial adhesive force, hold force, 180° peeling strength, cohesion, and permeability were measured. In addition, the contents of eucalyptol, camphor, and borneol in hydrogel transdermal patch were analyzed by GC. Results: The impacting factors which affected the patch shaping were in the order of glycerol > dihydroxyaluminium aminoacetate > EDTA > sodium polyacrylate NP-700. The optimized formulation was as following: 30% glycerol, 5% NP-700, 0.3% dihydroxyaluminium aminoacetate, and 0.03% EDTA. The permeation rates of eucalyptol, camphor, and borneol were 85.216, 4.442, and 3.941 μg/(cm2∙h), respectively. Conclusion: Emulsion-hydrogel transdermal patch of essential oil from Artemisia Argyi Folium has a better quality and a transdermal property of zero-order release process.

Improvement of preparing technique for compound glycyrrhiza oral solution / 国际药学研究杂志

Objective: To obtain a clear, well-tasted and qualified compound glycyrrhiza oral solution by improving the addi-tion method of compound camphor tincture. Methods: Pulvis Talci instead of 56% alcohol was used to improve the solubility of camphor and anise oil. Firstly, camphor and benzoic acid were dissolved in 95% alcohol. Then the anise oil was mixed with Pulvis Talci and triturated sufficiently. After that, camphor solution and water were mixed with Pulvis Talci and agitated sufficiently. The im-proved compound camphor tincture was obtained after filtration. At last, a new compound glycyrrhiza oral solution was obtained by the pharmacopeial method. Results: The preparation was clear, well-tasted and qualified. Conclusion: The improved method is fea-sible, simple, stabilized and economical.

Simultaneous Determination of Camphor and Menthol in Compound Diphenhydramine Liniment by GC / 中国药房

OBJECTIVE:To establish a method for simultaneous determination of camphor and menthol in Compound diphen-hydramine liniment. METHODS:GC was performed on the column of Agilent 19095N-123 INNOWAX capillary column,column temperature was 120 ℃,injection volume temperature was 220 ℃,FID detector was used with the temperature of 260 ℃,carrier gas was nitrogen gas,flow of column was 6.0 ml/min,air was 450 ml/min,hydrogen gas was 40 ml/min,split ratio was 20∶1 and injection volume was 1 μl. RESULTS:The linear range of mass concentration was 0.612-6.12 mg/ml(r=0.999 9)for camphor and 0.593-5.93 mg/ml(r=0.999 9)for menthol;RSDs of precision,stability and reproducibility tests were lower than 2%;the recov-eries were respectively 98.0%-100.7%(RSD=1.0%,n=6)and 98.7%-100.7%(RSD=0.7%,n=6). CONCLUSIONS:The meth-od is simple,accurate and reproducible,and can be used for the contents determination of camphor and menthol in Compound di-phenhydramine liniment.

Chemical resolution on (±)1-(Benzamidomethyl)-1,2,3,4-tetrahydro-isoquinoline / 中国生化药物杂志

Objective To obtain two types of optical isomers from 1-(Benzamidomethyl)-1,2,3,4-tetrahydro-isoquinoline (BTIQ). Methods ( ±) BTIQ as raw materials , optically pure camphor sulfonic acid as resolution agent was used and repeated resolution in acetone , And the resolution product was detected by specific optical rotation .The product of BTIQ was hydrolyzed , and the ratio of ATIQ was compared with that of the literature .ResuIts After two repeated chemical resolutions , the specific rotations of both enantiomers are no longer changed .It was showed that the products of higher optical purity.The specific rotation of both isomers are -35.65°(CH2Cl2, C=0.5)with the yield of 27.52%,and +35.17°(CH2Cl2, C =0.5) with the yield of 31.55% respectively.The specific rotation value of chiral 1,2,3,4-tetrahydroisoquino line ( ATIQ) which was the hydrolysis product of BTIQ consistent with values reported in the literature .ConcIusion The (-) BTIQ and ( +) BTIQ enantiomers were successfully obtained by the method of resolution , and the yield and optical purity of the obtained products are higher , laying the foundation for the further development of high efficiency , low toxicity of chiral schistosomicide ( praziquantel ) and other containing tetrahydroisoquinoline structure of chiral drugs .

Limit Test for Camphor in Shujin Huoxue Pills / 医药导报

Objective To establish a method for limit test of camphor in Shujin Huoxue pills. Methods A DB-WAX (30 m×0. 32 mm,0. 25 μm) capillary column was used with a programmed temperature. Results The linear range of camphor was 1. 05-210. 00 μg·mL-1(r=1. 0). The average recovery was 101. 7%(n=9, RSD=1. 2%). Conclusion The proposed method is simple, sensitive, accurate and reproducible, which is suitable for quality control of Shujin Huoxue Pills.

Simultaneous determination of camphor, isoborneol, L-borneol, β-caryophyllene and xanthoxylin in aifen by GC and hierarchical cluster analysis / 中国药学杂志

OBJECTIVE: To establish a GC method for simultaneous determination of camphor, isoborneol, L-borneol, β-caryo-phyllene and xanthoxylin in aifen, combined with hierarchical cluster analysis. METHODS: The GC analysis was carried out on HP-5 capillary column (30 m × 0.32 mm, 0.25 μm). Temperature programs; 90℃ (hold 2 min) programmed to 100℃ at 4℃ · min-1, then programmed to 160℃ (hold 6 min) at 20℃ · min-1. The detector was FID with 240℃. The inlet temperature was set at 240℃. The carrying gas was high-purity nitrogen (3.0 mL · min-1), split ratio was 50:1, injection volume was 0.5 μL. Cluster analysis was performed by SPSS16.0 software. RESULTS: The methodology validation for the assay of camphor, isoborneol, l-horneol, β-caryophyllene and xanthoxylin presented that they were in good liner correlation in the ranges of 0.02-0.32 (r=1.000 0), 0.01-0.08(r=1.000 0), 0.20-7.95(r=1.000 0), 0.01-0.40(r=1.0000), 0.08-0.67 mg · mL-1 (r=0.999 8), with the average recoveries (n=9) of 101.04% (RSD=1.04%), 99.08% (RSD=1.50%), 98.76% (RSD=1.67%), 99.85% (RSD=1.97%), 97.74% ( RSD=1.65%), respectively. The 24 batches of sample analyzed can be clustered into three classes according to the content of the five components. CONCLUSION: The developed method is simple, quick and accurate, which provides reference for the quality control of aifen.