| Objective: To establish a method for simultaneous determination of eucalyptol, limonene and α-pinene in Aningpai enteric soft capsules by HPLC-DAD,and determination of drug concentration of eucalyptol in plasma. Compare Myrtol Standardized Enteric Coated Sofe Capsules with Aningpai enteric soft capsule content differences.Method:1 To establish a method for simultaneous determination of eucalypt ol, limonene and α-pinene in Aningpai enteric soft capsules by HPLC-D AD.The determination was performed on ZORBAX SB-C18(4.6x150 m m, 5μm)column with mobile phase consisted of acetonitrile-water-isopropanol(70:28:2,V/V/V) and simultaneous determination of eucalyptol, limonene and α-pinene in Aningpai enteric soft capsules, and determination of drug concentration of eucalyptol in plasma.2 Comparison Aningpai enteric soft capsules and Myrtol standardized enteric coated soft capsule content differences: The determination was performed on ZORBAX SB-C18(4.6x150 mm, 5μm)column with mobile phase consisted of acetonitrile-water-isopropanol(70:28:2,V/V/V), simultaneous determination of eucalyptol, limonene and α-pinene in Aningpai enteric soft capsules and Myrtol standardized enteric coated soft capsule, and compare their differences.Results:1 To establish a method for simultaneous determination of eucalyptol, limonene and α-pinene in Aningpai enteric soft capsules by HPLCDAD. The determination was performed on ZORBAX SB-C18(4.6x150 m m, 5μm) column with mobile phase consisted of acetonitrile-water-isopropanol(70:28:2,V/V/V)at the flow rate of 1ml·min-1.The detection wavel-ength was set at 203 nm, and the column temperature was 40℃.The samples size was 10μl. In this conditions, eucalyptol, limonene and α-pinene was well separated, less impurity interference, R>1.5, The tR of eucalyptol, limonene and α-pinene were 3.9min, 9.5min and 11.9min respectively. Eucalyptol standard curve equation was Y=1163.5X-2.3028, r=0.9996(n=6), the linear ranges were 0.2~2.0mg·m L-1; limonene standard curve equation was Y=27002X+1774.6, r=0.9991(n=6), the linear ranges were 0.16~1.19mg·m L-1 and α-pinene standard curve equation was Y=23425X-109.11,r=0.9995(n=6), the linear ranges were 0.05~0.20mg·m L-1. Eucalyptol, limonene and α-pinene precision test of RSD were 1.7%(n=6), 0.26%(n=6), 0.3%(n=6);stability test of RSD were 2.4%(n=6), 0.6%(n=6), 1.1%(n=6); repeatability tests of RSD were 1.0%(n=6) and 0.9%(n=6) and 0.8%(n=6); the rate of recovery were eucalyptol 99.5%, RSD was 1.5%(n=6), limonene 99.2%, RSD was 1.4%(n=6), α-pinene 100.3%, RSD was 1.1%(n=6). In this conditions, eucalyptol and other peak was well separated, less impurity interference, the tR of eucalyptol is about 4.0min, the standard curve equation was Y=1827.1X-92.28, r=0.9991(n=6), the linear ranges were 0.10~2.0mg·m L-1. The extraction recovery of low, middle and high were 84.25%, 89.24% and 95.38%, RSD were 4.85%, 2.45% and 4.79%(n=3), respec-tively.2 The chromatographic conditions for determination of relatively Anningpai enteric soft capsule and Myrtol standardized enteric coated soft capsule content:The determination was performed on ZORBAX SB-C18(4.6x150 mm, 5μm)column with mobile phase consisted of acetonitrile-waterisopropanol(70:28:2,V/V/V)at the flow rate of 1ml·min-1.The detection wavelength was set at 203 nm, and the column temperature was 40℃.The samples size was 10μl. In this conditions, eucalyptol, limonene and α-pinene was well separated, less impurity interference, R>1.5, The tR of eucalyptol, limonene and α-pinene were 3.9min, 9.5min and 11.9min respectively. Eucalyptol standard curve equation was Y=1354.9X-39.468, r=0.9970(n=6), the linear ranges were 0.1~1.0mg·m L-1; limonene standard curve e-quation was Y=26518X+1510.9, r=0.9970(n=6), the linear ranges were 0.1~1.0mg·m L-1; α-pinene standard curve equation was Y=22491X- 5.2144, r=0.9999(n=6), the linear ranges were 0.025~0.5mg·m L-1. Three the precision test of RSD were 2%(n=6), 0.3%(n=6), 0.4%(n=6); stability test of RSD were 3.0%(n=6),0.5%(n=6), 0.6%(n=6); repeatability tests of RSD were 3.0%(n=6), 2.0%(n=6) and 1.8%(n=6); the rate of recovery were eucalyptol was 98.31%, RSD was 2.54%(n=6), limonene 97.29%, RSD was 2.04%(n=6), α-pinene 97.53%, RSD was 2.31%(n=6).Conclusion:1 To establish a method for simultaneous determination of eucalyptol, limonene and α-pinene in Aningpai enteric soft capsules by HPLC-DAD.This method is specificity and reproducible, high precision, simple and rapid, and suitable for quality control of Anningpai enteric soft capsules.2 The Anningpai enteric soft capsules and Myrtle standard enteric coated soft capsule containing eucalyptol, limonene and α-pinene, according to the test level of α=0.05, the content of eucalyptol in Myrtle Standard Enteric Coated Soft Capsule are higher than Anningpai Enteric Soft Capsules(P<0.05), others are no significant difference(P>0.05) between the Anningpai enteric soft capsule and Myrtol standardized enteric coated capsules. |
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