小中大按照这个条件做吧：
2.2. LC–MS–MS
An Applied Biosystems (Toronto, Canada) API 3000 triple-quadrupole tandem mass spectrometer, equipped with a Turbo Ionspray interface and an Agilent 1100 binary HPLC system, was used for LC–MS–MS analysis. The data were processed using Macquan software (PE Sciex). A Waters X-Terra™ RP C18 column (150 mm × 3.9 mm I.D., 5 μm particle size) was applied for the separation. The temperature of the column was set at 30 °C. The flow-rate was 500 μL/min, mobile phase component A was 3 mM CH3COONH4 (aq) and B was 3 mM CH3COONH4 acetonitrile, and the injection volume was 20 μL. The column was eluted with a linear gradient of 5–75% B over 0–8 min, 75–95% B over 8–10 min, and the composition was maintained 95% B for 2 min, then returned to 5% B at 12 min immediately. The LC effluent was split by the ratio of 4:1 using a valved three-way split, so that approximately 100 μL/min was introduced into the source of the mass spectrometry. The negative-ion mode of MS–MS was adopted and MRM was used for the specific detection of geniposide, baicaline, cholic acid and hyodeoxycholic acid. The ionspray voltage of −3500 V and ion source temperature of 350 °C were applied. The nebulizer gas (air) and curtain gas (nitrogen) were set at a value of 8 and 11 (instrument units), respectively. The flow-rate of drying gas (nitrogen) was 2 L/min. The dwell time was 200 ms. The optimized quad 2 rod offset (RO2) voltage, the quad 3 rod offset (RO3) voltage, stubbies 3 (ST3) voltage, orifice potential (OR) and ring focus voltage (RNG) are shown in Table 1. The collision gas (nitrogen) was set at 6 (instrument units), and the optimized collision energy (Q0-RO2) of 12 eV was used for geniposide, 30 eV for baicalin, 48 eV for cholic acid and 44 eV for hyodeoxycholic acid.
Simultaneous determination of geniposide, baicalin, cholic acid and hyodeoxycholic acid in rat serum for the pharmacokinetic investigations by high performance liquid chromatography–tandem mass spectrometry
Journal of Chromatography B
Volume 842, Issue 1, 14 September 2006, Pages 22-27
