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shweta ☆ 2009-10-08 15:37 (5712 d 18:13 ago) Posting: # 4321 Views: 5,622 |
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Dear sir, This is regarding the project that was carried out on instrument API 3000 and after then it has been transferred to API 3200. The calibration range has been changed from 50ng/mL-5000ng/mL to 10ng/mL - 5000ng/mL. After changing the instrument only specificity and one precision & accuracy batch has been submitted. My question is it sufficient to carry out only one P&A batch? Isn't there need of carry over and more P&A experiment?  Edit: Category changed. [Helmut] |
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Ohlbe ★★★ France, 2009-10-08 17:50 (5712 d 16:00 ago) @ shweta Posting: # 4323 Views: 5,047 |
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Dear Shweta, ❝ Dear sir, We also have some Ladies visiting the forum. Don't discourage them from answering  ❝ My question is it sufficient to carry out only one P&A batch? ❝ Isn't there need of caary over and more P&A experiment? One P&A batch is not sufficient. You have decreased the LLOQ from 50 to 10 ng/ml. You have to show P&A at the LLOQ level, both within-run and between-run. I think you also have to go for matrix effects again. API 3000 and 3200 have different ion sources (even if you have ESI on both instruments, the geometry of the source is different). Carry-over: IMHO this depends more on your HPLC system (autoinjector, injection valve, tubing etc.) than on the MS/MS system you have afterwards. Regards Ohlbe — Regards Ohlbe |
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shweta ☆ 2009-10-09 13:07 (5711 d 20:43 ago) @ Ohlbe Posting: # 4331 Views: 4,994 |
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Thank u very much sir, I'll ask u more question if i have any query. Edit: Full quote removed. Please delete anything from the text of the original poster which is not necessary in understanding your answer; see also this post! [Ohlbe] |
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moblak ☆ 2009-10-13 06:02 (5708 d 03:48 ago) @ shweta Posting: # 4345 Views: 4,911 |
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Dear Shweta ❝ The calibration range has been changed from 50ng/mL-5000ng/mL to 10ng/mL - 5000ng/mL. ❝ Isn't there need of carry over and more P&A experiment? IMHO you should also perform all stability experiments at the new (lower) QCL level. Regards Marko |
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shweta ☆ 2009-10-14 11:46 (5706 d 22:04 ago) @ moblak Posting: # 4351 Views: 4,790 |
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Dear Sir, This is in regarding to the stability study at newQC level. Why it should be carried out as new LQC having conc that is already proved in to previous calibration range. Edit: Full quote removed. Please delete anything from the text of the original poster which is not necessary in understanding your answer; see also this post! [Helmut] |
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Helmut ★★★   Vienna, Austria, 2009-10-14 14:44 (5706 d 19:06 ago) @ shweta Posting: # 4353 Views: 4,868 |
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Dear Shweta! ❝ Why it should be carried out as new LQC having conc that is already proved ❝ in to previous calibration range. I guess Marko was referring to FDA's guideline. Stability experiments shoud be carried out at the 'low and high concentrations' (Section IV.D. Stability, pp 6-7). The concentration of the low QC sample should lie 'within 3× the lower limit of quantification' (Section F. Specific Recommendations for Method Validation, p 13). Since you changed your LLOQ, your low QC should also move down. This requirement is reasonable, because for instance irreversible absorption to the container/stopper may hit you only at lower concentrations. — Dif-tor heh smusma 🖖🏼 Довге життя Україна! ![[image]](https://static.bebac.at/pics/Blue_and_yellow_ribbon_UA.png) Helmut Schütz ![[image]](https://static.bebac.at/img/CC by.png) The quality of responses received is directly proportional to the quality of the question asked. 🚮 Science Quotes |
Ing. Helmut Schütz