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Analysis of Steroidal Anti-Inflammatory Drugs Using LC/MS
Although steroidal anti-inflammatory drugs (adrenal steroidal anti-inflammatory drugs have been detected cortical hormones) have a very high anti-inflammatory in imported products labeled as “health foods” and it is efficacy, they are also known to have some side therefore important to monitor these drugs. An effects and it can be difficult to adjust their dosage to example of the analysis of steroidal anti-inflammatory an appropriate level. There are also reports that drugs performed using LC/MS is presented here.
When determining the LC/MS analytical conditions, it is necessary to consider both ionization (detection) and chromatographic separation. Because steroidal anti-inflammatory drugs have a low polarity, positive ion atmospheric pressure chemical ionization (APCI- Positive) was used. In general, using a methanol mobile phase in APCI gives a greater ionization efficiency than an acetonitrile mobile phase. In this analysis, however, an acetonitrile mobile phase was selected in order to improve the separation between dexamethasone (peak w) and betamethasone (peak e). Usually, it is said that 0.2 mL/min is an appropriate mobile phase flow rate for a column with an inner diameter of 2 mm. In this case, however, a mobile phase flow rate of 0.3 mL/min was used in order to reduce the analysis time. Even under these conditions, the column head pressure was 7.8 MPa. Fig.2 shows the SIM chromatograms obtained for Fig.1 Structures of Six Steroidal Anti-Inflammatory Drugs
Fig.2 SIM Chromatograms for Six Steroidal Anti-Inflammatory Drugs
In these mass spectra, in addition to protonated quantitative ions, and the other ions were used as molecules ([M+H]+), fragment ions ([M+H-H2O]+ and reference ions. Fig.3 shows the calibration curves [M+H-2×H2O]+), and mobile phase adduct protonated obtained by performing measurement 5 times at 6 molecules ([M+H+CH3CN]+) are observed. In this concentrations in the range 6.4 to 2,000 ng/mL. analysis, the ions were all monitored (Table 1), the Linearity (r2 > 0.9999) was attained over a relatively underlined protonated molecules were used as Fig.3 Calibration Curves for Six Steroidal Anti-Inflammatory Drugs (6.4 to 2,000 ng/mL) Area
Table 1 Analytical Conditions
: Phenomenex Synergi MAX-RP (2.0 mm I.D. × 150 mmL.) : 0.1% formic acid-water /acetonitrile (70:30) Mass number of monitor ions : m/z 402.1, 361.1, 343.1, 325.1 for prednisolone m/z 434.1, 393.1, 373.1, 355.1 for betamethasone & dexamethasone m/z 476.1, 435.1, 415.1 for triamcinolone acetonide m/z 494.1, 453.1, 413.1 for fluocinolone acetonide m/z 446.1, 405.1 for hydrocortisone acetate NOTES:
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