Gas chromatography of volatile oil Valerian Blackwater bornyl acetate content
【Abstract】 Objective To establish the essential oil of Valeriana Blackwater bornyl acetate method for the determination. Methods using gas chromatography, naphthalene
as the internal standard, DB-l7 capillary column, carrier gas
helium, electron impact (EI) ion source detector. The results of the chromatographic conditions, bornyl acetate in the sample volume 0.109 6 ~ 1.753 6 μg showed good linear
relationship within the framework of, r = 0.999 6; bornyl acetate recovery was 101.33%, RSD = 1.79%. Conclusion This method can accurately determine Blackwater Valerian volatile oil content of bornyl acetate.
Key words gas chromatography Blackwater Valerian essential
oil bornyl acetate
Determination of Bornyl Acetate in Valeriana amurensis Volatile Oil by Gas Chromatography
Abstract: ObjectiveTo establish the method for determination of bornyl acetate in Valeriana amurensis volatile oil by Gas Chromatography. MethodsThe GC system
consisted of DB-17capillary column, helium as the carrier gas and EI as the detector. Naphthalene was used as internal standard substance in the analysis method. ResultsThe standard curve of bornyl acetate was linear over the range of 0.109 6 ~
1.753 6 μg, r = 0.999 6. The mean recovery of bornyl acetate was 101.33%, RSD = 1.79%. ConclusionThe method can accurately determine the content of bornyl acetate in Valeriana amurensis volatile oil.
Key words: GC; Valeriana amurensis volatile oil; Bornyl
Blackwater is Valerianaceae Valerian Valeriana medicinal plants, with peace of mind God, rheumatism, blood lines, the analgesic efficacy, indications malaise, palpitations, insomnia, mania, dirty rash, rheumatism Bitong, Zhongwan
abdominal distension pain, dysmenorrhea, amenorrhea, bruises, [1 ~ 3]. Volatile oil component is Blackwater Valerian important material basis for efficacy, in which bornyl acetate as Valeriana essential oils and some Chinese characteristic
composition, have a calming, analgesic, anti-inflammation,
diarrhea and other pharmacological effects [4 ~ 6]. Wang Shumei, etc.  on the compound mixture of valerian bornyl acetate were qualitatively identified. However, on the genus Valeriana volatile oil content of bornyl acetate determination have not been reported, this experiment was established using gas chromatography bornyl acetate method for the determination, and different harvesting periods Blackwater Valerian Volatile oil, bornyl acetate were determined.
An instrument and reagent
QP5050A-type GC chromatography (Shimadzu, Japan); AB-N
Electronic Analytical Balance (Mettler - Toledo Instruments
Shanghai Co., Ltd.); micro-pipette (Dragon Medical Equipment
Blackwater Valerian samples (collected from Heilongjiang Province, Huma Daxinganling region, after all, Professor Xiaowei identified as genuine); bornyl acetate reference substance (China Pharmaceutical and Biological Products Institution, batch number 110759-200303); naphthalene,
methanol, for chromatography pure.
2 Methods and Results
2.1 Chromatographic conditions DB-17 fused silica
capillary column (30 m × 0.25 mm, 0.25 μm); carrier gas for
high-purity helium; flow rate of 20 ml / min; pre-column
pressure 63 kPa; initial temperature of 80 ? (keep 2 min ) to
3 ? / min rate up to 150 ? (to keep 3 min), followed by
10 ? / min rate up to 220 ? (to maintain 25 min);
gasification chamber temperature of 180 ?; electron impact
(EI) ion Source detector, electron energy 70 eV, accelerating
voltage of 0.8 kPa; detector temperature 250 ?; split ratio
of 20:1; the quality of scanning range 50 ~ 500 m / z; scanning speed 0.5 s / dec.
2.2 Preparation of test solution
2.2.1 Preparation of reference substance solution
precision that bornyl acetate take appropriate reference substance, add methanol produced 2.192 0 mg / ml solution.
2.2.2 Preparation of internal standard solution Weigh naphthalene precise amount, plus methanol produced 2.007 7 mg
/ ml solution.
2.2.3 Preparation for the test product solution, said amount to take Blackwater Valerian herbs, according to 2005 edition of "Chinese Pharmacopoeia" Appendix XD determination of volatile oil volatile oil extracted French, precision
drawing Blackwater Valerian Essential Oil 0.1 ml placed in 25 ml Flask , by adding internal standard solution, 5 ml, diluted with methanol to scale, shake.
2.3 The linear relationship between the study accurately draw reference substance solution 0.1,0.2,0.4,0.8,1.6 ml, were
placed in 2 ml flask, each internal standard solution, 0.4 ml, diluted with methanol to scale. Precision drawing were 1 μl,
into the gas chromatograph determination of sample volume by the reference substance and reference substance / internal standard peak area ratio of the regression, was standard
curve: Y = 0.406 5X-0.001 1, r = 0.999 6 (n = 5). The results show that bornyl acetate injection volume of 0.109 6 ~ 1.753 6 μg range a good linear relationship. Reposted elsewhere in the paper for free download http://
.4 Precision experiment to take the linear test items Xiadi 3:00 reference substance solution into the sample six consecutive times, the calculation reference substance and the internal standard peak area ratio of the average of 1.154 3, RSD = 0.69%.
2.5 to reproduce the experiment on the same batch of samples from the sampling start repeating measuring five times, measured the average level of 0.1382 g / ml, RSD = 2.04%.
2.6 Stability of test items for the experimental precision drawing solution of 1 μl, injection measurement,
recording the sample and the internal standard peak area ratio, at intervals of 1 h measured 1, 6 h in 7 times the average level measured 0.140 4 g / ml, RSD = 0.91%.
2.7 recoveries experimental precision drawing samples of known content of 5 copies of each adding a certain amount of bornyl acetate, measured and calculated recoveries. The results in Table 1. Table 1 The average recovery determination
2.8 Determination of sample taking valerian Blackwater samples from different collection periods 5 batches, according to test materials for the preparation of solutions prepared under the parallel solution of five samples, each sample
injection 1 μl, measured bornyl acetate content. The results shown in Table 2, chromatogram shown in Figure 1. Table 2 Sample assay results (omitted)
The method uses naphthalene as the internal standard, sensitive, accurate, reproducible, able to accurately determine Blackwater Valerian volatile oil content of bornyl acetate can be used for black water quality evaluation of medicinal Valerian.
Measurement results can be seen from the sample, different samples harvested during the volatile oil content of bornyl acetate slightly different, the highest value of fruit maturity, wilt phase content decreased. Therefore, if bornyl acetate content of quantitative indicators to assess the Blackwater Valerian essential oil, should be harvested fruit
maturity is the best.
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