Gas Chromatography of Foshan Renshenzaizaowan borneol content（气相色谱的佛山Renshenzaizaowan冰片含量）

1、 Gas Chromatography of Foshan Renshenzaizaowan borneol content Abstract Objective To establish the method of gas chromatography determination of the Foshan Renshenzaizaowan borneol content. Methods HP 5 fused silica capillary column (5% phenyl methyl siloxane (30.0 m 320 nm , 0.25 m film thickness c

2、olumn temperature was 110 C, into inlet temperature of 180 C, detector temperature of 250 C, nitrogen as a carrier gas. Results borneol the detection mass concentration in the range of 6.875 220.00 g / mL (r = 0.9999, n = 6) a good linear relationship, with an average recovery 98.59% (RSD = 1.52%).

3、Keywords: gas chromatography Foshan Renshenzaizaowan, borneol, Determination Abstract: Objective To establish a method for content determination of borneol in Foshanrenshenzaizao pills. Method The sample was analyzed on an HP 5 capillary column (5% phenyl methyl siloxane, 30.0 m 320 nm 0.25 m) using

4、 nitrogen as carrier gas. The temperatures of the column, injector and detector were 110, 180 and 250 , respectively.Result There was good linearity in the range of 6.88 220.00 g / mL (r = 0.9999, n = 6). The average recovery and relative standard deviation of borneol were 98.58% and 1.52%, respecti

5、vely. Conclusion This method is simple, accurate and reproducible for the quality control of Foshanrenshenzaizao pill. Keywords: gas chromatography; Foshanrenshenzaizao pill; borneol Foshan Renshenzaizaowan compound formed by ginseng, artificial bezoar, dragons blood, Angelica, the borneol (syntheti

6、c campholytic), rhubarb, with Qufeng stasis the efficacy Huoxuetongluo for stroke, walks with difficulty, eye and mouth skewed, hand, foot cramps, left paralyzed right numbness of the limbs, aching pain, hemiplegia, slurred speech 1. prescription borneol (synthetic campholytic) is blindly commonly u

7、sed drugs, the San Yu fire, heat, swelling and other effects. borneol (synthetic borneol) the main component of each other isomers borneol and Isoborneol its chemical structure characteristic UV absorption, thin layer scanning method and gas chromatography 2-4 is the determination of such compounds

8、better method. established Gas Chromatography content of Foshan Renshenzaizaowan borneol, the method is simple, without interference of impurities, separation is good, the results are accurate, can be used as one of the quality control of the preparation method. 1 instrument and reagent Agilent HP68

9、90 gas chromatograph the, HP Chemstatations workstations, FID detector, CQ 250 ultrasonic processor (Shanghai, power 250 W, frequency of 33 kHz. Borneol (China Pharmaceutical and Biological Products, batch number: 110881200504, methyl salicylate (China Pharmaceutical and Biological Products, batch n

10、umber: 7078702, the Foshan Renshenzaizaowan total of 10 batches (Foshan Feng Pharmaceutical company), other reagents used were of analytical grade. 2 Methods and Results 2.1 Chromatographic conditions and system suitability test Column HP 5 fused silica capillary column (5% phenyl methyl siloxane (3

11、0.0 m 320 nm , 0.25 m film thickness, the column temperature was 110 C inlet temperature of 180 C, detector temperature of 250 C. The carrier gas was high purity nitrogen split ratio of 20:1, the chromatographic conditions, borneol, methyl salicylate (internal standard), the number of theoretical pl

12、ates is greater than 40,000. borneol and methyl salicylate (internal standard) The degree of separation is greater than 2. 2.2 Preparation of the solution 2.2.1 internal standard solution preparation water accurately weighed Yang Methyl right amount placed in 1 000 mL volumetric flask, add ethanol t

13、o a concentration of 0.130 0 mg / mL solution, shake, that is, too. 2.2.2 control solution preparation accurately weighed borneol appropriate reference substance placed in a 100 mL volumetric flask, plus the internal standard solution dissolved and diluted to a concentration of 0.090 0 mg / mL solut

14、ion, shake, that is, too. 2.2.3 for the Preparation of the test solution to take this product into pieces, taking about 2 g, accurately weighed, plus diatomite 2 g pestle, placed in a stoppered conical flask, precision by adding 25 mL of the internal standard solution Mesa, said that given the weigh

15、t, ultrasound treatment for 30 min, let cool, and then said that given the weight, reduce the weight of ethanol complement the filtrate obtained, that is, too. 2.3 Method for determination Drawing reference solution into the gas chromatograph according to the above chromatographic conditions, borneo

16、l and methyl salicylate peak area was measured and calculated correction factor, to learn the test solution into the gas chromatograph above chromatographic conditions, in terms of the internal standard method was . 2.4 linear relationship between Precision Weigh borneol appropriate reference substa

17、nce, the internal standard solution was diluted to the mark, shake, to a concentration of 220.00 g / mL control solution borneol precision drawing 5 mL of the reference solution placed in a 10 mL volumetric flask , plus the internal standard solution was diluted to scale, shake, having a concentrati

18、on of 110.00 g / mL control solution borneol, ibid progressively diluted with the internal standard solution formulated six different concentration gradient 220.00,110.00,55.00,27.50 to learn the solution 13.75,6.875 g / mL reference solution. injection according to the above chromatographic conditi

19、ons, and record the peak area, and borneol mass concentration () as abscissa, the borneol peak area of the internal standard peak area than (A) for the vertical axis, linear regression to obtain the regression equation A = 0.012 4 0.015 1 (r = 0.999 9, n = 6) The results showed that borneol the dete

20、ction mass concentration in the range of 6.875 220.00 g / mL insider sexual relations. 2.5 negative interference investigation Takes on the default the borneol prescription, preparation process made negative, “2.2.3” method plus ethanol ultrasonic extraction obtained negative control solution. Were

21、drawn for the test solution, reference solution, negative control solution into the chromatographic conditions sample analysis results show that the other herbs and accessories borneol determination of non-interference, as shown in Figure 1. Links to free papers Download Center Figure 1 Gas chromato

22、gram slightly 2.6 instrument precision test Take the same test solution (batch GC0007 according to the above chromatographic conditions, repeated injections six times measured borneol content results borneol content RSD 1.02%, indicating good precision instrument. 2.7 Stability Test Take the same te

23、st solution, the chromatographic conditions were 0,1,2,4,6,8 h sample measured, calculated the borneol peak area of the internal standard peak area ratio of 1.69% RSD results show that for The test solution is stable within 8 h. 2.8 Repeatability test 5 copies of each of the samples accurately weigh

24、ed the same batch (batch GC0007) 2 g, “2.2.3” method to obtain the test solution, determination of each copy of the test content, results an average of 0.5972 mg / g, RSD = 1.09%. The results show that this Law repeatability. 2.9 The average recovery test Have measured the content of the sample (bat

25、ch GC0007, bornyl mass ratio of 0.597 2 mg/g6 1 g, accurately weighed, 1 g, were added diatomite pestle, adding precision borneol Markers solution (mass concentration of 0.6017 mg/mL1 mL, “2.2.3” method to obtain the test solution measured an average recovery of 98.59%, RSD 1.52%. 2.10 sample determ

26、ination 10 batches of samples, respectively, according to the preparation of the test solution was prepared for the test solution, according to the determination of “2.3” items, the results are shown in Table 1. Table 110 batches of samples measured results slightly 3 Discussion 3.1 References 2-4 E

27、xtraction solvent selection with ethanol, ethyl acetate and chloroform, etc., the selection of the internal standard substance of naphthalene and methyl salicylate. Trials comparing pestle, add celite, and ethanol as extraction solvent ultrasonic extraction (power 250 W, frequency 33 kHz, methyl sal

28、icylate as an internal standard, borneol extract significantly increased the toxicity of ethanol, and less irritating, lower prices and methyl salicylate, borneol have a good separation, and so the use of ethanol as extracting solvent, ultrasonic extraction, and methyl salicylate as the internal standard method. 3.2 by ultrasonic extraction method, try a different extraction time (20 min, 30 min, 40 min samples were extracted, 30 mi