A method for detecting impurity cis-perhydroisoindole in mitiglinide calcium
A technology of mitiglinide calcium and perhydroisoindole, which is applied in the field of medicine to achieve the effects of strong specificity and improved drug safety
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Embodiment 1
[0030] 1 Instruments and materials
[0031] 1.1 Instruments: Triple Quad4500 mass spectrometer (AB, USA), LC20A high performance liquid chromatograph (Shimadzu, Japan);
[0032] 1.2 Reagents: Methanol and acetonitrile are of mass spectrometry grade, acetic acid (chromatographic grade), and water is ultrapure water.
[0033] 2 Methods and results
[0034] 2.1 Chromatography and mass spectrometry conditions
[0035] Chromatographic column: MGⅢC 18 (2.0×100mm, 3μm, Shiseido), flow rate: 0.1ml / min, column temperature: 40°C, injection volume: 1μl, mobile phase: acetonitrile (containing 0.1% acetic acid)-water (containing 0.1% acetic acid). The gradient elution table is shown in Table 3.
[0036] Table 3 Gradient elution table
[0037]
[0038] Ion source: electrospray ionization source (ESI), positive ion mode: select multiple reaction detection scanning (MRM) mode, spray voltage (IS) 5500V; drying gas temperature 550 ° C; atomization gas (Gas1) 50psi; auxiliary gas (Gas2 ...
Embodiment 2
[0066] Embodiment 2: the detection of actual sample
[0067] 1) Get the former medicine of mitiglinide calcium, dissolve or constant volume with methanol, be mixed with the solution that contains 0.5mg mitiglinide calcium in 1ml, as need testing solution;
[0068] 2) Take the test solution prepared in step 1), adopt the same instruments and reagents as in Example 1, and carry out LC-MS / MS detection according to the chromatographic and mass spectrometry conditions shown in step 1) 2.1.
[0069] 3) According to the standard curve obtained in Example 1, find out the impurity cis-perhydroisoindole content in mitiglinide calcium.
[0070] Adopt above-mentioned method to detect three batches of samples, the result is as follows:
[0071] Table 8 Test results
[0072] Sample lot number 1 2 3 cis perhydroisoindole content% 0.016 0.015 0.013
[0073] .
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